# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1841201'
_audit_update_record             
;
2018-05-03 deposited with the CCDC.
2018-06-25 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT971_shelx               
;
PROBLEM: Check Calcd Resid. Dens.  1.07A   From I1              4.07 eA-3
RESPONSE: Absorption problems with  crystals - best result presented
;
# Added during the CSD deposition process: Thursday 03 May 2018 11:08 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H18 Ca N2 O6, 2(I)'
_chemical_formula_sum            'C6 H18 Ca I2 N2 O6'
_chemical_formula_weight         508.10

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   4.9952(4)
_cell_length_b                   5.9493(5)
_cell_length_c                   13.8126(12)
_cell_angle_alpha                95.593(13)
_cell_angle_beta                 90.980(12)
_cell_angle_gamma                90.965(11)
_cell_volume                     408.40(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    820
_cell_measurement_theta_min      1.5
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.066
_exptl_crystal_F_000             242
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_exptl_absorpt_coefficient_mu    4.178
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.697
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
'The program SADABS-2008/1 - G.M. Sheldrick was used to apply a multi-scan absorption correction.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Tube'
_diffrn_measurement_device_type  'Rigaku Mercury2 (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 13.6612
_diffrn_reflns_number            4214
_diffrn_reflns_av_unetI/netI     0.0736
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.482
_diffrn_reflns_theta_max         27.466
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1859
_reflns_number_gt                1381
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1859
_refine_ls_number_parameters     96
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_gt           0.0659
_refine_ls_wR_factor_ref         0.1743
_refine_ls_wR_factor_gt          0.1615
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_restrained_S_all      1.106
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.05875(14) 0.78223(11) 0.15666(5) 0.0393(3) Uani 1 1 d . . . . .
Ca1 Ca 1.0000 0.5000 0.5000 0.0327(6) Uani 1 2 d S . P . .
O2 O 0.2441(13) 0.3537(12) 0.3663(5) 0.0374(16) Uani 1 1 d . . . . .
O1 O 0.6398(15) 0.2795(13) 0.4319(5) 0.0415(17) Uani 1 1 d . . . . .
N1 N 0.4114(16) 0.2911(14) 0.1829(6) 0.0298(16) Uani 1 1 d . . . . .
O3 O 1.115(2) 0.1923(17) 0.5913(7) 0.062(2) Uani 1 1 d D . . . .
C2 C 0.610(2) 0.2849(18) 0.2618(7) 0.035(2) Uani 1 1 d . . . . .
H1 H 0.7418 0.4052 0.2576 0.041 Uiso 1 1 calc R U . . .
H2 H 0.7025 0.1424 0.2537 0.041 Uiso 1 1 calc R U . . .
C1 C 0.4855(19) 0.3114(15) 0.3616(7) 0.0305(19) Uani 1 1 d . . . . .
C3 C 0.526(2) 0.2707(18) 0.0849(7) 0.038(2) Uani 1 1 d . . . . .
H5 H 0.6713 0.3779 0.0829 0.058 Uiso 1 1 calc R U . . .
H7 H 0.3907 0.3001 0.0379 0.058 Uiso 1 1 calc R U . . .
H6 H 0.5915 0.1206 0.0701 0.058 Uiso 1 1 calc R U . . .
H3 H 0.31(2) 0.428(18) 0.190(7) 0.02(2) Uiso 1 1 d . . . . .
H4 H 0.28(2) 0.166(16) 0.185(7) 0.02(2) Uiso 1 1 d . . . . .
H8 H 1.279(5) 0.210(14) 0.580(6) 0.004(19) Uiso 1 1 d D . . . .
H9 H 1.04(2) 0.31(4) 0.58(4) 0.5(5) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ca1 O2 2.335(6) 2_666 ?
Ca1 O2 2.335(6) 1_655 ?
Ca1 O1 2.338(7) . ?
Ca1 O1 2.338(7) 2_766 ?
Ca1 O3 2.394(10) 2_766 ?
Ca1 O3 2.394(10) . ?
Ca1 H8 2.56(8) . ?
Ca1 H9 1.6(2) . ?
O2 C1 1.238(11) . ?
O2 Ca1 2.335(6) 1_455 ?
O1 C1 1.261(12) . ?
N1 C2 1.465(13) . ?
N1 C3 1.474(13) . ?
N1 H3 0.97(11) . ?
N1 H4 0.99(10) . ?
O3 H8 0.843(10) . ?
O3 H9 0.839(10) . ?
C2 C1 1.517(13) . ?
C2 H1 0.9700 . ?
C2 H2 0.9700 . ?
C3 H5 0.9600 . ?
C3 H7 0.9600 . ?
C3 H6 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ca1 O2 180.0 2_666 1_655 ?
O2 Ca1 O1 93.5(3) 2_666 . ?
O2 Ca1 O1 86.5(3) 1_655 . ?
O2 Ca1 O1 86.5(3) 2_666 2_766 ?
O2 Ca1 O1 93.5(3) 1_655 2_766 ?
O1 Ca1 O1 180.0(3) . 2_766 ?
O2 Ca1 O3 92.3(3) 2_666 2_766 ?
O2 Ca1 O3 87.7(3) 1_655 2_766 ?
O1 Ca1 O3 91.9(3) . 2_766 ?
O1 Ca1 O3 88.1(3) 2_766 2_766 ?
O2 Ca1 O3 87.7(3) 2_666 . ?
O2 Ca1 O3 92.3(3) 1_655 . ?
O1 Ca1 O3 88.1(3) . . ?
O1 Ca1 O3 91.9(3) 2_766 . ?
O3 Ca1 O3 180.0(5) 2_766 . ?
O2 Ca1 H8 99.7(16) 2_666 . ?
O2 Ca1 H8 80.3(16) 1_655 . ?
O1 Ca1 H8 102.2(14) . . ?
O1 Ca1 H8 77.8(14) 2_766 . ?
O3 Ca1 H8 160.8(7) 2_766 . ?
O3 Ca1 H8 19.2(7) . . ?
O2 Ca1 H9 77(10) 2_666 . ?
O2 Ca1 H9 103(10) 1_655 . ?
O1 Ca1 H9 88(10) . . ?
O1 Ca1 H9 92(10) 2_766 . ?
O3 Ca1 H9 169(10) 2_766 . ?
O3 Ca1 H9 11(10) . . ?
H8 Ca1 H9 28(5) . . ?
C1 O2 Ca1 129.1(6) . 1_455 ?
C1 O1 Ca1 129.9(7) . . ?
C2 N1 C3 114.0(7) . . ?
C2 N1 H3 112(6) . . ?
C3 N1 H3 108(6) . . ?
C2 N1 H4 110(6) . . ?
C3 N1 H4 107(5) . . ?
H3 N1 H4 105(8) . . ?
Ca1 O3 H8 91(6) . . ?
Ca1 O3 H9 22(10) . . ?
H8 O3 H9 106(3) . . ?
N1 C2 C1 112.5(8) . . ?
N1 C2 H1 109.1 . . ?
C1 C2 H1 109.1 . . ?
N1 C2 H2 109.1 . . ?
C1 C2 H2 109.1 . . ?
H1 C2 H2 107.8 . . ?
O2 C1 O1 126.3(9) . . ?
O2 C1 C2 118.0(9) . . ?
O1 C1 C2 115.7(8) . . ?
N1 C3 H5 109.5 . . ?
N1 C3 H7 109.5 . . ?
H5 C3 H7 109.5 . . ?
N1 C3 H6 109.5 . . ?
H5 C3 H6 109.5 . . ?
H7 C3 H6 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H3 I1 0.97(11) 2.54(11) 3.483(8) 163(8) .
N1 H4 I1 0.99(10) 2.51(10) 3.462(9) 161(8) 1_545

_refine_diff_density_max         3.985
_refine_diff_density_min         -0.925
_refine_diff_density_rms         0.282

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1841213'
_audit_update_record             
;
2018-05-03 deposited with the CCDC.
2018-06-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C9 H25 Mg N3 O8, 2(Br)'
_chemical_formula_sum            'C9 H25 Br2 Mg N3 O8'
_chemical_formula_weight         487.45

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   9.6161(8)
_cell_length_b                   18.9415(18)
_cell_length_c                   9.9930(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1820.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    872
_cell_measurement_theta_min      2.0
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.779
_exptl_crystal_F_000             984
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_exptl_absorpt_coefficient_mu    4.528
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.692
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
'The program SADABS-2008/1 - G.M. Sheldrick was used to apply a multi-scan absorption correction.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Tube'
_diffrn_measurement_device_type  'Rigaku Mercury2 (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 13.6612
_diffrn_reflns_number            5918
_diffrn_reflns_av_unetI/netI     0.0831
_diffrn_reflns_av_R_equivalents  0.0977
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.150
_diffrn_reflns_theta_max         27.504
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measured_fraction_theta_full 0.940
_diffrn_reflns_Laue_measured_fraction_max 0.907
_diffrn_reflns_Laue_measured_fraction_full 0.940
_diffrn_reflns_point_group_measured_fraction_max 0.907
_diffrn_reflns_point_group_measured_fraction_full 0.940
_reflns_number_total             1952
_reflns_number_gt                1033
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1952
_refine_ls_number_parameters     166
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1277
_refine_ls_R_factor_gt           0.0506
_refine_ls_wR_factor_ref         0.1662
_refine_ls_wR_factor_gt          0.1188
_refine_ls_goodness_of_fit_ref   0.892
_refine_ls_restrained_S_all      0.892
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br -0.00602(9) 0.90715(4) 0.73409(7) 0.0394(3) Uani 1 1 d . . . . .
Mg1 Mg 0.4143(3) 0.7500 0.2183(3) 0.0201(7) Uani 1 2 d S T P . .
O3 O 0.3053(5) 0.6684(2) 0.1233(4) 0.0228(10) Uani 1 1 d . . . . .
O2 O 0.0476(7) 0.7500 0.4494(6) 0.0251(15) Uani 1 2 d S T P . .
O5 O 0.5241(5) 0.8273(2) 0.3221(4) 0.0255(11) Uani 1 1 d D . . . .
O4 O 0.4635(5) 0.5815(2) 0.1269(5) 0.0313(12) Uani 1 1 d . . . . .
O1 O 0.2578(7) 0.7500 0.3528(6) 0.0316(17) Uani 1 2 d S T P . .
N1 N 0.1416(11) 0.7500 0.6978(9) 0.033(2) Uani 1 2 d S T P . .
N2 N 0.3088(8) 0.4918(3) -0.0109(6) 0.0303(14) Uani 1 1 d . . . . .
C1 C 0.1766(11) 0.7500 0.4520(9) 0.023(2) Uani 1 2 d S T P . .
C4 C 0.3476(7) 0.6069(3) 0.0989(6) 0.0223(15) Uani 1 1 d . . . . .
C5 C 0.2422(8) 0.5576(4) 0.0370(8) 0.0291(17) Uani 1 1 d . . . . .
C2 C 0.2465(11) 0.7500 0.5897(10) 0.029(2) Uani 1 2 d S T P . .
C6 C 0.2063(10) 0.4404(4) -0.0690(9) 0.039(2) Uani 1 1 d . . . . .
C3 C 0.2096(17) 0.7500 0.8345(11) 0.050(3) Uani 1 2 d S T P . .
H1 H 0.320(8) 0.708(4) 0.602(7) 0.04(2) Uiso 1 1 d . . . . .
H2 H 0.091(10) 0.716(4) 0.694(9) 0.07(3) Uiso 1 1 d . . . . .
H3 H 0.258(9) 0.702(5) 0.844(11) 0.08(4) Uiso 1 1 d . . . . .
H4 H 0.131(13) 0.7500 0.897(13) 0.05(4) Uiso 1 2 d S . P . .
H5 H 0.205(6) 0.579(3) -0.042(5) 0.001(13) Uiso 1 1 d . . . . .
H6 H 0.148(10) 0.543(5) 0.080(9) 0.08(3) Uiso 1 1 d . . . . .
H7 H 0.372(10) 0.503(5) -0.063(10) 0.06(3) Uiso 1 1 d . . . . .
H8 H 0.356(9) 0.460(5) 0.064(8) 0.06(3) Uiso 1 1 d . . . . .
H9 H 0.163(7) 0.466(4) -0.139(7) 0.03(2) Uiso 1 1 d . . . . .
H10 H 0.155(8) 0.431(3) 0.009(8) 0.03(2) Uiso 1 1 d . . . . .
H11 H 0.256(6) 0.402(4) -0.096(7) 0.019(18) Uiso 1 1 d . . . . .
H12 H 0.623(2) 0.823(3) 0.340(5) 0.009(15) Uiso 1 1 d D . . . .
H13 H 0.527(12) 0.870(4) 0.268(11) 0.13(5) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mg1 O1 2.018(7) . ?
Mg1 O5 2.083(5) 7_575 ?
Mg1 O5 2.083(5) . ?
Mg1 O3 2.094(5) 7_575 ?
Mg1 O3 2.094(5) . ?
Mg1 O2 2.110(7) 6_656 ?
O3 C4 1.259(7) . ?
O2 C1 1.240(11) . ?
O2 Mg1 2.110(7) 6_556 ?
O5 H12 0.97(2) . ?
O5 H13 0.98(2) . ?
O4 C4 1.246(8) . ?
O1 C1 1.262(11) . ?
N1 C2 1.478(14) . ?
N1 C3 1.515(14) . ?
N1 H2 0.81(8) . ?
N2 C5 1.482(9) . ?
N2 C6 1.502(10) . ?
N2 H7 0.83(9) . ?
N2 H8 1.06(9) . ?
C1 C2 1.532(13) . ?
C4 C5 1.510(10) . ?
C5 H5 0.96(5) . ?
C5 H6 1.04(10) . ?
C2 H1 1.08(7) . ?
C6 H9 0.95(7) . ?
C6 H10 0.94(7) . ?
C6 H11 0.91(7) . ?
C3 H3 1.02(9) . ?
C3 H4 0.98(13) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Mg1 O5 92.6(2) . 7_575 ?
O1 Mg1 O5 92.6(2) . . ?
O5 Mg1 O5 89.4(3) 7_575 . ?
O1 Mg1 O3 85.9(2) . 7_575 ?
O5 Mg1 O3 176.7(2) 7_575 7_575 ?
O5 Mg1 O3 87.76(17) . 7_575 ?
O1 Mg1 O3 85.9(2) . . ?
O5 Mg1 O3 87.76(17) 7_575 . ?
O5 Mg1 O3 176.7(2) . . ?
O3 Mg1 O3 95.0(3) 7_575 . ?
O1 Mg1 O2 169.2(3) . 6_656 ?
O5 Mg1 O2 95.0(2) 7_575 6_656 ?
O5 Mg1 O2 95.0(2) . 6_656 ?
O3 Mg1 O2 86.80(19) 7_575 6_656 ?
O3 Mg1 O2 86.80(19) . 6_656 ?
C4 O3 Mg1 127.5(4) . . ?
C1 O2 Mg1 128.6(6) . 6_556 ?
Mg1 O5 H12 122(3) . . ?
Mg1 O5 H13 109(7) . . ?
H12 O5 H13 98(8) . . ?
C1 O1 Mg1 170.0(7) . . ?
C2 N1 C3 111.3(10) . . ?
C2 N1 H2 112(7) . . ?
C3 N1 H2 107(7) . . ?
C5 N2 C6 112.8(7) . . ?
C5 N2 H7 108(6) . . ?
C6 N2 H7 114(7) . . ?
C5 N2 H8 116(5) . . ?
C6 N2 H8 101(5) . . ?
H7 N2 H8 106(8) . . ?
O2 C1 O1 127.1(8) . . ?
O2 C1 C2 117.2(8) . . ?
O1 C1 C2 115.7(9) . . ?
O4 C4 O3 127.1(6) . . ?
O4 C4 C5 117.0(6) . . ?
O3 C4 C5 115.8(6) . . ?
N2 C5 C4 111.3(6) . . ?
N2 C5 H5 104(3) . . ?
C4 C5 H5 110(3) . . ?
N2 C5 H6 106(5) . . ?
C4 C5 H6 126(5) . . ?
H5 C5 H6 97(6) . . ?
N1 C2 C1 110.9(8) . . ?
N1 C2 H1 112(4) . . ?
C1 C2 H1 113(4) . . ?
N2 C6 H9 104(4) . . ?
N2 C6 H10 98(4) . . ?
H9 C6 H10 119(6) . . ?
N2 C6 H11 107(4) . . ?
H9 C6 H11 115(6) . . ?
H10 C6 H11 112(6) . . ?
N1 C3 H3 106(6) . . ?
N1 C3 H4 104(7) . . ?
H3 C3 H4 107(6) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H2 Br1 0.81(8) 2.54(8) 3.318(5) 161(9) 7_575
N2 H7 Br1 0.83(9) 2.68(10) 3.437(7) 152(8) 4_565
N2 H8 Br1 1.06(9) 2.44(9) 3.487(7) 167(7) 8_655

_refine_diff_density_max         0.529
_refine_diff_density_min         -0.791
_refine_diff_density_rms         0.129

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1841207'
_audit_update_record             
;
2018-05-03 deposited with the CCDC.
2018-06-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C9 H21 Ca N3 O6, 2(Br)'
_chemical_formula_sum            'C9 H21 Br2 Ca N3 O6'
_chemical_formula_weight         467.19

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   9.2414(6)
_cell_length_b                   17.6966(13)
_cell_length_c                   10.3565(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1693.7(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    817
_cell_measurement_theta_min      2.0
_cell_measurement_theta_max      27.5

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.832
_exptl_crystal_F_000             936
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.063
_exptl_absorpt_coefficient_mu    5.115
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.803
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
'The program SADABS-2008/1 - G.M. Sheldrick was used to apply a multi-scan absorption correction.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Tube'
_diffrn_measurement_device_type  'Rigaku Mercury2 (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 13.6612
_diffrn_reflns_number            16686
_diffrn_reflns_av_unetI/netI     0.0725
_diffrn_reflns_av_R_equivalents  0.1593
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.279
_diffrn_reflns_theta_max         27.593
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2017
_reflns_number_gt                1002
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2017
_refine_ls_number_parameters     149
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1348
_refine_ls_R_factor_gt           0.0499
_refine_ls_wR_factor_ref         0.1790
_refine_ls_wR_factor_gt          0.1264
_refine_ls_goodness_of_fit_ref   0.945
_refine_ls_restrained_S_all      0.945
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.00751(8) 0.08326(4) 0.72032(7) 0.0385(3) Uani 1 1 d . . . . .
Ca1 Ca 0.46541(18) 0.2500 0.22187(18) 0.0221(4) Uani 1 2 d S T P . .
O3 O 0.8398(5) 0.3534(3) 0.3730(5) 0.0468(14) Uani 1 1 d . . . . .
O2 O 0.1009(7) 0.2500 0.4714(6) 0.0371(17) Uani 1 2 d S T P . .
O1 O 0.3317(8) 0.2500 0.4088(7) 0.053(2) Uani 1 2 d S T P . .
O4 O 0.6084(6) 0.3396(3) 0.3172(6) 0.0528(15) Uani 1 1 d . . . . .
N1 N 0.1642(8) 0.2500 0.7227(8) 0.0293(18) Uani 1 2 d S T P . .
N2 N 0.7940(6) 0.4857(3) 0.4909(6) 0.0298(14) Uani 1 1 d . . . . .
C4 C 0.7105(7) 0.3726(4) 0.3702(7) 0.0322(17) Uani 1 1 d . . . . .
C1 C 0.2329(10) 0.2500 0.4902(10) 0.033(2) Uani 1 2 d S T P . .
C5 C 0.6683(7) 0.4434(4) 0.4430(8) 0.0303(16) Uani 1 1 d . . . . .
C2 C 0.2829(10) 0.2500 0.6284(10) 0.027(2) Uani 1 2 d S T P . .
C6 C 0.7542(11) 0.5543(5) 0.5642(10) 0.049(2) Uani 1 1 d . . . . .
C3 C 0.2105(14) 0.2500 0.8585(10) 0.043(3) Uani 1 2 d S T P . .
H1 H 0.330(6) 0.291(3) 0.647(6) 0.013(15) Uiso 1 1 d . . . . .
H2 H 0.103(7) 0.293(4) 0.707(6) 0.029(18) Uiso 1 1 d . . . . .
H3 H 0.268(11) 0.291(6) 0.879(11) 0.11(4) Uiso 1 1 d . . . . .
H4 H 0.12(2) 0.2500 0.94(2) 0.19(9) Uiso 1 2 d S . P . .
H5 H 0.614(7) 0.428(3) 0.521(7) 0.028(18) Uiso 1 1 d . . . . .
H6 H 0.615(7) 0.476(4) 0.388(7) 0.033(19) Uiso 1 1 d . . . . .
H7 H 0.856(7) 0.452(4) 0.545(7) 0.033(19) Uiso 1 1 d . . . . .
H8 H 0.845(7) 0.496(4) 0.420(8) 0.04(2) Uiso 1 1 d . . . . .
H9 H 0.695(7) 0.537(4) 0.638(7) 0.03(2) Uiso 1 1 d . . . . .
H10 H 0.689(12) 0.579(6) 0.514(13) 0.10(4) Uiso 1 1 d . . . . .
H11 H 0.838(9) 0.575(4) 0.586(8) 0.05(2) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ca1 O4 2.288(5) . ?
Ca1 O4 2.288(5) 7_565 ?
Ca1 O1 2.296(7) . ?
Ca1 O2 2.361(7) 6_656 ?
Ca1 O3 2.379(5) 4_455 ?
Ca1 O3 2.379(5) 6_556 ?
O3 C4 1.243(8) . ?
O3 Ca1 2.379(5) 6_656 ?
O2 C1 1.235(11) . ?
O2 Ca1 2.361(7) 6_556 ?
O1 C1 1.244(12) . ?
O4 C4 1.238(8) . ?
N1 C2 1.468(12) . ?
N1 C3 1.471(13) . ?
N1 H2 0.96(6) . ?
N2 C5 1.469(8) . ?
N2 C6 1.478(10) . ?
N2 H7 1.00(7) . ?
N2 H8 0.89(8) . ?
C4 C5 1.513(10) . ?
C1 C2 1.504(15) . ?
C5 H5 0.98(7) . ?
C5 H6 0.95(7) . ?
C2 H1 0.87(6) . ?
C6 H9 0.99(7) . ?
C6 H10 0.91(11) . ?
C6 H11 0.89(8) . ?
C3 H3 0.93(10) . ?
C3 H4 1.2(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Ca1 O4 87.8(3) . 7_565 ?
O4 Ca1 O1 86.9(2) . . ?
O4 Ca1 O1 86.9(2) 7_565 . ?
O4 Ca1 O2 93.43(19) . 6_656 ?
O4 Ca1 O2 93.43(19) 7_565 6_656 ?
O1 Ca1 O2 179.5(3) . 6_656 ?
O4 Ca1 O3 173.2(2) . 4_455 ?
O4 Ca1 O3 85.8(2) 7_565 4_455 ?
O1 Ca1 O3 94.90(19) . 4_455 ?
O2 Ca1 O3 84.77(17) 6_656 4_455 ?
O4 Ca1 O3 85.8(2) . 6_556 ?
O4 Ca1 O3 173.2(2) 7_565 6_556 ?
O1 Ca1 O3 94.90(19) . 6_556 ?
O2 Ca1 O3 84.77(17) 6_656 6_556 ?
O3 Ca1 O3 100.5(3) 4_455 6_556 ?
C4 O3 Ca1 132.1(5) . 6_656 ?
C1 O2 Ca1 131.1(7) . 6_556 ?
C1 O1 Ca1 165.3(7) . . ?
C4 O4 Ca1 163.4(5) . . ?
C2 N1 C3 114.8(8) . . ?
C2 N1 H2 109(4) . . ?
C3 N1 H2 109(4) . . ?
C5 N2 C6 113.3(6) . . ?
C5 N2 H7 110(4) . . ?
C6 N2 H7 110(4) . . ?
C5 N2 H8 104(5) . . ?
C6 N2 H8 112(5) . . ?
H7 N2 H8 106(6) . . ?
O4 C4 O3 127.9(7) . . ?
O4 C4 C5 114.5(6) . . ?
O3 C4 C5 117.6(6) . . ?
O2 C1 O1 128.2(10) . . ?
O2 C1 C2 117.0(9) . . ?
O1 C1 C2 114.8(8) . . ?
N2 C5 C4 112.8(6) . . ?
N2 C5 H5 106(4) . . ?
C4 C5 H5 108(4) . . ?
N2 C5 H6 108(4) . . ?
C4 C5 H6 110(4) . . ?
H5 C5 H6 112(6) . . ?
N1 C2 C1 113.7(8) . . ?
N1 C2 H1 103(4) . . ?
C1 C2 H1 111(4) . . ?
N2 C6 H9 106(4) . . ?
N2 C6 H10 106(8) . . ?
H9 C6 H10 104(9) . . ?
N2 C6 H11 105(5) . . ?
H9 C6 H11 115(7) . . ?
H10 C6 H11 121(8) . . ?
N1 C3 H3 113(7) . . ?
N1 C3 H4 117(10) . . ?
H3 C3 H4 105(9) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H2 Br1 0.96(6) 2.36(6) 3.287(3) 160(5) 7_565
N2 H7 Br1 1.00(7) 2.38(7) 3.321(6) 157(5) 7_665
N2 H8 Br1 0.89(8) 2.52(7) 3.336(7) 153(6) 3_656

_refine_diff_density_max         1.110
_refine_diff_density_min         -0.907
_refine_diff_density_rms         0.136

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 1841210'
_audit_update_record             
;
2018-05-03 deposited with the CCDC.
2018-06-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H28 Ca N4 O8, 2(I), 2(H2O)'
_chemical_formula_sum            'C12 H32 Ca I2 N4 O10'
_chemical_formula_weight         686.29

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   11.2880(8)
_cell_length_b                   10.0620(7)
_cell_length_c                   23.0573(16)
_cell_angle_alpha                90
_cell_angle_beta                 103.722(4)
_cell_angle_gamma                90
_cell_volume                     2544.1(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    921
_cell_measurement_theta_min      1.8
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.792
_exptl_crystal_F_000             1352
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.236
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.112
_exptl_absorpt_coefficient_mu    2.722
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.740
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
'The program SADABS-2008/1 - G.M. Sheldrick was used to apply a multi-scan absorption correction.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Tube'
_diffrn_measurement_device_type  'Rigaku Mercury2 (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 13.6612
_diffrn_reflns_number            25445
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_av_R_equivalents  0.0639
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.864
_diffrn_reflns_theta_max         27.513
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5835
_reflns_number_gt                4163
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5835
_refine_ls_number_parameters     393
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0392
_refine_ls_wR_factor_ref         0.1279
_refine_ls_wR_factor_gt          0.1050
_refine_ls_goodness_of_fit_ref   0.878
_refine_ls_restrained_S_all      0.878
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.27522(3) 0.48884(3) 0.72558(2) 0.03339(12) Uani 1 1 d . . . . .
I2 I 0.78542(4) 0.92530(3) 0.76287(2) 0.03778(12) Uani 1 1 d . . . . .
Ca1 Ca 0.5000 0.5000 0.5000 0.0178(2) Uani 1 2 d S . P . .
Ca2 Ca 0.5000 1.0000 0.5000 0.0179(2) Uani 1 2 d S . P . .
O1 O 0.3567(3) 0.4599(3) 0.55548(15) 0.0276(7) Uani 1 1 d . . . . .
O2 O 0.5554(3) 0.6809(3) 0.56082(14) 0.0236(6) Uani 1 1 d . . . . .
O3 O 0.3464(3) 0.6306(3) 0.43551(15) 0.0283(7) Uani 1 1 d . . . . .
O4 O 0.6387(3) 1.0783(3) 0.44930(16) 0.0299(8) Uani 1 1 d . . . . .
O5 O 0.6552(3) 0.8737(3) 0.56638(15) 0.0275(7) Uani 1 1 d . . . . .
O6 O 0.4502(3) 0.8196(3) 0.43565(14) 0.0247(7) Uani 1 1 d . . . . .
O7 O 0.1599(3) 0.4065(4) 0.5218(2) 0.0448(10) Uani 1 1 d . . . . .
O8 O 0.8301(3) 1.0278(4) 0.44743(17) 0.0337(8) Uani 1 1 d . . . . .
O9 O 0.0777(4) 0.6416(5) 0.4681(2) 0.0493(11) Uani 1 1 d . . . . .
O10 O 0.9361(4) 0.9302(4) 0.55975(19) 0.0417(10) Uani 1 1 d . . . . .
N1 N 0.4008(4) 0.2727(5) 0.6381(2) 0.0293(9) Uani 1 1 d . . . . .
N2 N 0.8624(4) 0.7731(4) 0.63727(19) 0.0246(8) Uani 1 1 d . . . . .
N3 N 0.1378(4) 0.7313(4) 0.36793(18) 0.0238(8) Uani 1 1 d . . . . .
N4 N 0.6248(4) 1.2863(4) 0.3732(2) 0.0286(9) Uani 1 1 d . . . . .
C1 C 0.2638(4) 0.3895(5) 0.5547(2) 0.0272(10) Uani 1 1 d . . . . .
C2 C 0.2795(5) 0.2706(5) 0.5963(2) 0.0321(11) Uani 1 1 d . . . . .
C3 C 0.4296(8) 0.1515(6) 0.6751(3) 0.0477(16) Uani 1 1 d . . . . .
C4 C 0.6487(4) 0.7537(4) 0.57657(18) 0.0191(8) Uani 1 1 d . . . . .
C5 C 0.7622(4) 0.6816(5) 0.6098(2) 0.0257(9) Uani 1 1 d . . . . .
C6 C 0.9766(5) 0.7009(7) 0.6643(3) 0.0388(12) Uani 1 1 d . . . . .
C7 C 0.3533(4) 0.7497(4) 0.42344(19) 0.0212(8) Uani 1 1 d . . . . .
C8 C 0.2403(4) 0.8232(5) 0.3904(2) 0.0253(9) Uani 1 1 d . . . . .
C9 C 0.0253(5) 0.8006(6) 0.3353(3) 0.0339(11) Uani 1 1 d . . . . .
C10 C 0.7359(4) 1.0972(5) 0.43381(19) 0.0234(9) Uani 1 1 d . . . . .
C11 C 0.7434(5) 1.2178(5) 0.3949(2) 0.0289(10) Uani 1 1 d . . . . .
C12 C 0.5377(5) 1.2169(6) 0.3251(3) 0.0348(11) Uani 1 1 d . . . . .
H1 H 0.283(5) 0.194(6) 0.577(3) 0.034(15) Uiso 1 1 d . . . . .
H2 H 0.222(4) 0.270(5) 0.622(2) 0.019(12) Uiso 1 1 d . . . . .
H3 H 0.450(7) 0.280(8) 0.616(3) 0.06(2) Uiso 1 1 d . . . . .
H4 H 0.412(6) 0.334(7) 0.659(3) 0.05(2) Uiso 1 1 d . . . . .
H5 H 0.419(6) 0.076(7) 0.645(3) 0.048(18) Uiso 1 1 d . . . . .
H6 H 0.373(5) 0.150(6) 0.698(3) 0.035(16) Uiso 1 1 d . . . . .
H7 H 0.507(9) 0.167(10) 0.699(5) 0.10(3) Uiso 1 1 d . . . . .
H8 H 0.791(5) 0.619(6) 0.583(3) 0.039(16) Uiso 1 1 d . . . . .
H9 H 0.747(4) 0.636(5) 0.637(2) 0.016(12) Uiso 1 1 d . . . . .
H10 H 0.874(5) 0.825(6) 0.609(3) 0.028(14) Uiso 1 1 d . . . . .
H11 H 0.845(6) 0.811(7) 0.663(3) 0.045(19) Uiso 1 1 d . . . . .
H12 H 1.000(7) 0.659(7) 0.639(3) 0.05(2) Uiso 1 1 d . . . . .
H13 H 0.952(5) 0.632(6) 0.690(3) 0.036(15) Uiso 1 1 d . . . . .
H14 H 1.041(7) 0.756(8) 0.683(3) 0.06(2) Uiso 1 1 d . . . . .
H15 H 0.212(6) 0.883(6) 0.416(3) 0.041(17) Uiso 1 1 d . . . . .
H16 H 0.261(6) 0.865(7) 0.362(3) 0.050(19) Uiso 1 1 d . . . . .
H17 H 0.120(4) 0.706(5) 0.398(2) 0.015(12) Uiso 1 1 d . . . . .
H18 H 0.156(5) 0.678(6) 0.345(3) 0.031(15) Uiso 1 1 d . . . . .
H19 H 0.007(5) 0.864(6) 0.363(3) 0.036(15) Uiso 1 1 d . . . . .
H20 H 0.042(6) 0.847(7) 0.306(3) 0.044(18) Uiso 1 1 d . . . . .
H21 H -0.036(6) 0.742(7) 0.319(3) 0.052(19) Uiso 1 1 d . . . . .
H22 H 0.795(6) 1.281(7) 0.418(3) 0.045(17) Uiso 1 1 d . . . . .
H23 H 0.766(5) 1.186(6) 0.361(3) 0.039(16) Uiso 1 1 d . . . . .
H24 H 0.601(6) 1.298(7) 0.403(3) 0.045(19) Uiso 1 1 d . . . . .
H25 H 0.638(6) 1.365(8) 0.359(3) 0.05(2) Uiso 1 1 d . . . . .
H26 H 0.503(5) 1.139(6) 0.339(2) 0.029(14) Uiso 1 1 d . . . . .
H27 H 0.568(6) 1.198(7) 0.297(3) 0.046(18) Uiso 1 1 d . . . . .
H28 H 0.477(6) 1.267(7) 0.306(3) 0.049(18) Uiso 1 1 d . . . . .
H29 H 0.000(8) 0.620(8) 0.464(4) 0.06(2) Uiso 1 1 d . . . . .
H30 H 0.091(6) 0.560(7) 0.487(3) 0.045(18) Uiso 1 1 d . . . . .
H31 H 1.010(6) 0.929(5) 0.552(3) 0.028(14) Uiso 1 1 d . . . . .
H32 H 0.895(7) 0.948(7) 0.525(3) 0.05(2) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ca1 O2 2.292(3) 3_666 ?
Ca1 O2 2.292(3) . ?
Ca1 O1 2.323(3) . ?
Ca1 O1 2.323(3) 3_666 ?
Ca1 O3 2.392(3) 3_666 ?
Ca1 O3 2.392(3) . ?
Ca2 O4 2.304(3) . ?
Ca2 O4 2.304(3) 3_676 ?
Ca2 O6 2.328(3) 3_676 ?
Ca2 O6 2.328(3) . ?
Ca2 O5 2.399(3) 3_676 ?
Ca2 O5 2.399(3) . ?
O1 C1 1.263(6) . ?
O2 C4 1.264(5) . ?
O3 C7 1.237(5) . ?
O4 C10 1.246(5) . ?
O5 C4 1.236(5) . ?
O6 C7 1.275(5) . ?
O7 C1 1.248(6) . ?
O8 C10 1.248(6) . ?
O9 H29 0.89(8) . ?
O9 H30 0.92(7) . ?
O10 H31 0.89(6) . ?
O10 H32 0.84(8) . ?
N1 C2 1.476(7) . ?
N1 C3 1.480(7) . ?
N1 H3 0.84(8) . ?
N1 H4 0.77(7) . ?
N2 C5 1.479(6) . ?
N2 C6 1.482(7) . ?
N2 H10 0.87(6) . ?
N2 H11 0.76(7) . ?
N3 C8 1.475(6) . ?
N3 C9 1.487(7) . ?
N3 H17 0.82(5) . ?
N3 H18 0.81(6) . ?
N4 C12 1.471(7) . ?
N4 C11 1.483(7) . ?
N4 H24 0.81(7) . ?
N4 H25 0.89(8) . ?
C1 C2 1.517(7) . ?
C2 H1 0.90(6) . ?
C2 H2 0.97(5) . ?
C3 H5 1.02(7) . ?
C3 H6 0.92(7) . ?
C3 H7 0.93(9) . ?
C4 C5 1.512(6) . ?
C5 H8 0.99(6) . ?
C5 H9 0.83(5) . ?
C6 H12 0.81(8) . ?
C6 H13 0.99(6) . ?
C6 H14 0.93(8) . ?
C7 C8 1.514(6) . ?
C8 H15 0.95(7) . ?
C8 H16 0.87(7) . ?
C9 H19 0.95(6) . ?
C9 H20 0.88(7) . ?
C9 H21 0.92(7) . ?
C10 C11 1.524(7) . ?
C11 H22 0.93(7) . ?
C11 H23 0.94(6) . ?
C12 H26 0.97(6) . ?
C12 H27 0.83(7) . ?
C12 H28 0.88(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ca1 O2 180.0 3_666 . ?
O2 Ca1 O1 94.27(12) 3_666 . ?
O2 Ca1 O1 85.73(12) . . ?
O2 Ca1 O1 85.73(12) 3_666 3_666 ?
O2 Ca1 O1 94.27(12) . 3_666 ?
O1 Ca1 O1 180.0 . 3_666 ?
O2 Ca1 O3 89.78(11) 3_666 3_666 ?
O2 Ca1 O3 90.21(11) . 3_666 ?
O1 Ca1 O3 93.37(12) . 3_666 ?
O1 Ca1 O3 86.63(12) 3_666 3_666 ?
O2 Ca1 O3 90.21(11) 3_666 . ?
O2 Ca1 O3 89.79(11) . . ?
O1 Ca1 O3 86.63(12) . . ?
O1 Ca1 O3 93.37(12) 3_666 . ?
O3 Ca1 O3 180.00(13) 3_666 . ?
O4 Ca2 O4 180.0 . 3_676 ?
O4 Ca2 O6 88.08(12) . 3_676 ?
O4 Ca2 O6 91.92(12) 3_676 3_676 ?
O4 Ca2 O6 91.92(12) . . ?
O4 Ca2 O6 88.08(12) 3_676 . ?
O6 Ca2 O6 180.0 3_676 . ?
O4 Ca2 O5 88.66(12) . 3_676 ?
O4 Ca2 O5 91.34(12) 3_676 3_676 ?
O6 Ca2 O5 91.31(11) 3_676 3_676 ?
O6 Ca2 O5 88.69(11) . 3_676 ?
O4 Ca2 O5 91.34(12) . . ?
O4 Ca2 O5 88.66(12) 3_676 . ?
O6 Ca2 O5 88.69(11) 3_676 . ?
O6 Ca2 O5 91.31(11) . . ?
O5 Ca2 O5 180.00(13) 3_676 . ?
C1 O1 Ca1 140.8(3) . . ?
C4 O2 Ca1 136.3(3) . . ?
C7 O3 Ca1 126.7(3) . . ?
C10 O4 Ca2 161.5(3) . . ?
C4 O5 Ca2 124.9(3) . . ?
C7 O6 Ca2 129.5(3) . . ?
H29 O9 H30 83(6) . . ?
H31 O10 H32 99(6) . . ?
C2 N1 C3 114.1(5) . . ?
C2 N1 H3 104(5) . . ?
C3 N1 H3 110(5) . . ?
C2 N1 H4 114(5) . . ?
C3 N1 H4 109(5) . . ?
H3 N1 H4 105(7) . . ?
C5 N2 C6 112.1(4) . . ?
C5 N2 H10 107(4) . . ?
C6 N2 H10 110(4) . . ?
C5 N2 H11 109(5) . . ?
C6 N2 H11 106(5) . . ?
H10 N2 H11 113(7) . . ?
C8 N3 C9 112.8(4) . . ?
C8 N3 H17 103(3) . . ?
C9 N3 H17 103(3) . . ?
C8 N3 H18 110(4) . . ?
C9 N3 H18 107(4) . . ?
H17 N3 H18 120(6) . . ?
C12 N4 C11 114.9(4) . . ?
C12 N4 H24 115(5) . . ?
C11 N4 H24 104(5) . . ?
C12 N4 H25 106(5) . . ?
C11 N4 H25 109(5) . . ?
H24 N4 H25 108(7) . . ?
O7 C1 O1 126.1(5) . . ?
O7 C1 C2 116.4(4) . . ?
O1 C1 C2 117.4(4) . . ?
N1 C2 C1 110.7(4) . . ?
N1 C2 H1 101(4) . . ?
C1 C2 H1 111(4) . . ?
N1 C2 H2 105(3) . . ?
C1 C2 H2 113(3) . . ?
H1 C2 H2 115(5) . . ?
N1 C3 H5 104(4) . . ?
N1 C3 H6 105(4) . . ?
H5 C3 H6 113(6) . . ?
N1 C3 H7 105(6) . . ?
H5 C3 H7 118(7) . . ?
H6 C3 H7 111(7) . . ?
O5 C4 O2 126.5(4) . . ?
O5 C4 C5 118.9(4) . . ?
O2 C4 C5 114.6(4) . . ?
N2 C5 C4 112.9(4) . . ?
N2 C5 H8 110(4) . . ?
C4 C5 H8 111(3) . . ?
N2 C5 H9 107(3) . . ?
C4 C5 H9 111(3) . . ?
H8 C5 H9 106(5) . . ?
N2 C6 H12 111(5) . . ?
N2 C6 H13 105(3) . . ?
H12 C6 H13 104(6) . . ?
N2 C6 H14 114(5) . . ?
H12 C6 H14 106(6) . . ?
H13 C6 H14 116(5) . . ?
O3 C7 O6 125.5(4) . . ?
O3 C7 C8 119.7(4) . . ?
O6 C7 C8 114.8(4) . . ?
N3 C8 C7 111.6(4) . . ?
N3 C8 H15 105(4) . . ?
C7 C8 H15 112(4) . . ?
N3 C8 H16 112(4) . . ?
C7 C8 H16 106(4) . . ?
H15 C8 H16 111(6) . . ?
N3 C9 H19 106(4) . . ?
N3 C9 H20 109(4) . . ?
H19 C9 H20 106(6) . . ?
N3 C9 H21 112(4) . . ?
H19 C9 H21 115(5) . . ?
H20 C9 H21 108(6) . . ?
O4 C10 O8 126.7(4) . . ?
O4 C10 C11 117.8(4) . . ?
O8 C10 C11 115.6(4) . . ?
N4 C11 C10 113.4(4) . . ?
N4 C11 H22 105(4) . . ?
C10 C11 H22 109(4) . . ?
N4 C11 H23 106(4) . . ?
C10 C11 H23 107(4) . . ?
H22 C11 H23 117(5) . . ?
N4 C12 H26 113(3) . . ?
N4 C12 H27 112(5) . . ?
H26 C12 H27 111(6) . . ?
N4 C12 H28 114(4) . . ?
H26 C12 H28 108(5) . . ?
H27 C12 H28 99(6) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H4 I1 0.77(7) 2.89(8) 3.487(5) 137(6) .
N2 H11 I2 0.76(7) 2.80(7) 3.561(4) 174(7) .
N3 H18 I2 0.81(6) 2.85(6) 3.612(4) 157(5) 4_575
N4 H25 I1 0.89(8) 2.79(8) 3.577(5) 148(6) 3_676

_refine_diff_density_max         1.368
_refine_diff_density_min         -1.022
_refine_diff_density_rms         0.146

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC4
_database_code_depnum_ccdc_archive 'CCDC 1841208'
_audit_update_record             
;
2018-05-03 deposited with the CCDC.
2018-06-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C9 H21 Ca0.61 N3 O6 Sr0.4, 2(Cl)'
_chemical_formula_sum            'C9 H21 Br2 Ca0.61 N3 O6 Sr0.40'
_chemical_formula_weight         486.60

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sr Sr -1.5307 3.2498 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   9.1728(7)
_cell_length_b                   17.8422(14)
_cell_length_c                   10.4200(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1705.4(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    847
_cell_measurement_theta_min      2.0
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.895
_exptl_crystal_F_000             966
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    6.201
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.784
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
'The program SADABS-2008/1 - G.M. Sheldrick was used to apply a multi-scan absorption correction.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Tube'
_diffrn_measurement_device_type  'Rigaku Mercury2 (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 13.6612
_diffrn_reflns_number            16650
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_av_R_equivalents  0.0841
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.263
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2020
_reflns_number_gt                1275
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2020
_refine_ls_number_parameters     150
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0787
_refine_ls_R_factor_gt           0.0384
_refine_ls_wR_factor_ref         0.1421
_refine_ls_wR_factor_gt          0.1120
_refine_ls_goodness_of_fit_ref   0.895
_refine_ls_restrained_S_all      0.895
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.99351(5) 0.91675(2) 0.27709(5) 0.0270(2) Uani 1 1 d . . . . .
Ca1 Ca 0.53033(11) 0.7500 0.77516(9) 0.0234(4) Uani 0.605(6) 2 d S T P . .
Sr1 Sr 0.53033(11) 0.7500 0.77516(9) 0.0234(4) Uani 0.395(6) 2 d S T P . .
O1 O 0.8981(6) 0.7500 0.5229(5) 0.0382(12) Uani 1 2 d S T P . .
O2 O 0.6657(6) 0.7500 0.5844(5) 0.0523(16) Uani 1 2 d S T P . .
O3 O 0.1478(5) 0.6409(2) 0.6280(4) 0.0543(12) Uani 1 1 d . . . . .
O4 O 0.3786(5) 0.6620(2) 0.6791(4) 0.0640(13) Uani 1 1 d . . . . .
N1 N 0.8364(6) 0.7500 0.2719(5) 0.0260(12) Uani 1 2 d S T P . .
N2 N 0.2039(5) 0.5115(2) 0.5072(4) 0.0297(9) Uani 1 1 d . . . . .
C1 C 0.7677(8) 0.7500 0.5029(7) 0.0302(16) Uani 1 2 d S T P . .
C2 C 0.7136(8) 0.7500 0.3646(7) 0.0269(15) Uani 1 2 d S T P . .
C3 C 0.7886(10) 0.7500 0.1360(7) 0.0335(17) Uani 1 2 d S T P . .
C4 C 0.2790(6) 0.6257(3) 0.6282(5) 0.0337(12) Uani 1 1 d . . . . .
C5 C 0.3279(5) 0.5564(3) 0.5570(5) 0.0266(10) Uani 1 1 d . . . . .
C6 C 0.2501(7) 0.4433(3) 0.4360(6) 0.0397(14) Uani 1 1 d . . . . .
H1 H 0.651(5) 0.708(3) 0.348(5) 0.035(14) Uiso 1 1 d . . . . .
H2 H 0.891(6) 0.712(3) 0.284(5) 0.040(16) Uiso 1 1 d . . . . .
H3 H 0.729(6) 0.708(4) 0.128(6) 0.052(18) Uiso 1 1 d . . . . .
H4 H 0.864(8) 0.7500 0.085(8) 0.04(2) Uiso 1 2 d S . P . .
H5 H 0.383(6) 0.573(3) 0.478(5) 0.032(14) Uiso 1 1 d . . . . .
H6 H 0.383(5) 0.523(3) 0.614(5) 0.024(12) Uiso 1 1 d . . . . .
H7 H 0.140(7) 0.546(4) 0.459(6) 0.063(19) Uiso 1 1 d . . . . .
H8 H 0.147(5) 0.498(3) 0.580(5) 0.029(13) Uiso 1 1 d . . . . .
H9 H 0.305(6) 0.457(3) 0.356(6) 0.047(17) Uiso 1 1 d . . . . .
H10 H 0.309(6) 0.409(3) 0.496(7) 0.052(19) Uiso 1 1 d . . . . .
H11 H 0.171(7) 0.416(3) 0.418(6) 0.049(18) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ca1 O4 2.324(4) 7_575 ?
Ca1 O4 2.324(4) . ?
Ca1 O2 2.344(5) . ?
Ca1 O1 2.428(5) 6_557 ?
Ca1 O3 2.444(4) 4_566 ?
Ca1 O3 2.444(4) 6_657 ?
Ca1 Sr1 4.6163(4) 6_557 ?
Ca1 Sr1 4.6163(4) 6_657 ?
O1 C1 1.214(8) . ?
O1 Sr1 2.428(5) 6_657 ?
O1 Ca1 2.428(5) 6_657 ?
O2 C1 1.263(8) . ?
O3 C4 1.233(6) . ?
O3 Sr1 2.444(4) 6_557 ?
O3 Ca1 2.444(4) 6_557 ?
O4 C4 1.239(6) . ?
N1 C3 1.482(9) . ?
N1 C2 1.483(9) . ?
N1 H2 0.85(5) . ?
N2 C5 1.485(6) . ?
N2 C6 1.487(7) . ?
N2 H7 0.98(7) . ?
N2 H8 0.95(5) . ?
C1 C2 1.525(10) . ?
C1 Sr1 3.339(8) 6_657 ?
C2 H1 0.96(5) . ?
C3 H3 0.93(6) . ?
C3 H4 0.87(8) . ?
C4 C5 1.510(8) . ?
C4 Sr1 3.337(6) 6_557 ?
C5 H5 1.01(6) . ?
C5 H6 0.98(5) . ?
C6 H9 1.00(6) . ?
C6 H10 1.03(6) . ?
C6 H11 0.90(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Ca1 O4 84.9(2) 7_575 . ?
O4 Ca1 O2 87.24(16) 7_575 . ?
O4 Ca1 O2 87.24(16) . . ?
O4 Ca1 O1 94.25(15) 7_575 6_557 ?
O4 Ca1 O1 94.25(15) . 6_557 ?
O2 Ca1 O1 178.0(2) . 6_557 ?
O4 Ca1 O3 84.49(17) 7_575 4_566 ?
O4 Ca1 O3 168.52(17) . 4_566 ?
O2 Ca1 O3 96.69(14) . 4_566 ?
O1 Ca1 O3 82.10(12) 6_557 4_566 ?
O4 Ca1 O3 168.52(17) 7_575 6_657 ?
O4 Ca1 O3 84.48(16) . 6_657 ?
O2 Ca1 O3 96.69(13) . 6_657 ?
O1 Ca1 O3 82.10(12) 6_557 6_657 ?
O3 Ca1 O3 105.7(2) 4_566 6_657 ?
O4 Ca1 Sr1 49.92(13) 7_575 6_557 ?
O4 Ca1 Sr1 49.92(13) . 6_557 ?
O2 Ca1 Sr1 115.47(16) . 6_557 ?
O1 Ca1 Sr1 66.56(13) 6_557 6_557 ?
O3 Ca1 Sr1 119.02(11) 4_566 6_557 ?
O3 Ca1 Sr1 119.02(11) 6_657 6_557 ?
O4 Ca1 Sr1 123.09(13) 7_575 6_657 ?
O4 Ca1 Sr1 123.09(13) . 6_657 ?
O2 Ca1 Sr1 51.49(15) . 6_657 ?
O1 Ca1 Sr1 126.49(13) 6_557 6_657 ?
O3 Ca1 Sr1 66.96(11) 4_566 6_657 ?
O3 Ca1 Sr1 66.96(11) 6_657 6_657 ?
Sr1 Ca1 Sr1 166.95(4) 6_557 6_657 ?
C1 O1 Sr1 129.8(5) . 6_657 ?
C1 O1 Ca1 129.8(5) . 6_657 ?
Sr1 O1 Ca1 0.0 6_657 6_657 ?
C1 O2 Ca1 164.2(5) . . ?
C4 O3 Sr1 127.2(4) . 6_557 ?
C4 O3 Ca1 127.2(4) . 6_557 ?
Sr1 O3 Ca1 0.0 6_557 6_557 ?
C4 O4 Ca1 168.2(4) . . ?
C3 N1 C2 113.4(6) . . ?
C3 N1 H2 108(4) . . ?
C2 N1 H2 110(4) . . ?
C5 N2 C6 113.5(4) . . ?
C5 N2 H7 107(4) . . ?
C6 N2 H7 115(4) . . ?
C5 N2 H8 106(3) . . ?
C6 N2 H8 110(3) . . ?
H7 N2 H8 104(5) . . ?
O1 C1 O2 127.9(7) . . ?
O1 C1 C2 118.9(6) . . ?
O2 C1 C2 113.2(7) . . ?
O1 C1 Sr1 33.9(3) . 6_657 ?
O2 C1 Sr1 94.0(5) . 6_657 ?
C2 C1 Sr1 152.8(5) . 6_657 ?
N1 C2 C1 111.6(6) . . ?
N1 C2 H1 109(3) . . ?
C1 C2 H1 112(3) . . ?
N1 C3 H3 105(4) . . ?
N1 C3 H4 110(5) . . ?
H3 C3 H4 114(4) . . ?
O3 C4 O4 127.2(5) . . ?
O3 C4 C5 117.9(5) . . ?
O4 C4 C5 114.8(5) . . ?
O3 C4 Sr1 35.7(3) . 6_557 ?
O4 C4 Sr1 91.6(4) . 6_557 ?
C5 C4 Sr1 153.6(3) . 6_557 ?
N2 C5 C4 112.7(4) . . ?
N2 C5 H5 105(3) . . ?
C4 C5 H5 108(3) . . ?
N2 C5 H6 106(3) . . ?
C4 C5 H6 110(3) . . ?
H5 C5 H6 114(4) . . ?
N2 C6 H9 111(4) . . ?
N2 C6 H10 109(4) . . ?
H9 C6 H10 112(5) . . ?
N2 C6 H11 109(4) . . ?
H9 C6 H11 111(5) . . ?
H10 C6 H11 103(5) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H2 Br1 0.85(5) 2.48(5) 3.306(3) 163(5) 7_575
N2 H7 Br1 0.98(7) 2.42(7) 3.334(5) 154(5) 7_475
N2 H8 Br1 0.95(5) 2.45(5) 3.345(5) 158(4) 3_646

_refine_diff_density_max         0.694
_refine_diff_density_min         -0.906
_refine_diff_density_rms         0.107

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC5
_database_code_depnum_ccdc_archive 'CCDC 1841202'
_audit_update_record             
;
2018-05-03 deposited with the CCDC.
2018-06-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H18 Ca N2 O6, 2(I)'
_chemical_formula_sum            'C6 H18 Ca I2 N2 O6'
_chemical_formula_weight         508.10

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   5.0003(5)
_cell_length_b                   5.9936(6)
_cell_length_c                   13.8450(15)
_cell_angle_alpha                95.502(19)
_cell_angle_beta                 91.031(19)
_cell_angle_gamma                91.228(17)
_cell_volume                     412.84(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    830
_cell_measurement_theta_min      1.5
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.044
_exptl_crystal_F_000             242
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    4.133
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.553
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
'The program SADABS-2008/1 - G.M. Sheldrick was used to apply a multi-scan absorption correction.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Tube'
_diffrn_measurement_device_type  'Rigaku Mercury2 (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 13.6612
_diffrn_reflns_number            4252
_diffrn_reflns_av_unetI/netI     0.1161
_diffrn_reflns_av_R_equivalents  0.0864
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.478
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             1884
_reflns_number_gt                1049
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1884
_refine_ls_number_parameters     96
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0886
_refine_ls_R_factor_gt           0.0422
_refine_ls_wR_factor_ref         0.1271
_refine_ls_wR_factor_gt          0.1041
_refine_ls_goodness_of_fit_ref   0.640
_refine_ls_restrained_S_all      0.640
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.05798(11) 0.78215(8) 0.15820(5) 0.0528(2) Uani 1 1 d . . . . .
Ca1 Ca 1.0000 0.5000 0.5000 0.0422(5) Uani 1 2 d S . P . .
O1 O 0.6392(11) 0.2825(10) 0.4321(4) 0.0513(14) Uani 1 1 d . . . . .
O2 O 0.2434(10) 0.3543(10) 0.3667(4) 0.0484(13) Uani 1 1 d . . . . .
C1 C 0.4834(14) 0.3100(12) 0.3619(5) 0.0372(16) Uani 1 1 d . . . . .
C2 C 0.6064(15) 0.2833(13) 0.2627(5) 0.0408(16) Uani 1 1 d . . . . .
H1 H 0.7408 0.4011 0.2588 0.049 Uiso 1 1 calc R U . . .
H2 H 0.6955 0.1408 0.2546 0.049 Uiso 1 1 calc R U . . .
N1 N 0.4100(12) 0.2923(10) 0.1837(4) 0.0376(13) Uani 1 1 d D . . . .
C3 C 0.5242(18) 0.2710(14) 0.0850(6) 0.050(2) Uani 1 1 d . . . . .
H5 H 0.6456 0.3948 0.0787 0.075 Uiso 1 1 calc R U . . .
H7 H 0.3824 0.2714 0.0373 0.075 Uiso 1 1 calc R U . . .
H6 H 0.6185 0.1331 0.0751 0.075 Uiso 1 1 calc R U . . .
O3 O 1.1149(18) 0.1967(14) 0.5906(6) 0.083(2) Uani 1 1 d D . . . .
H3 H 0.313(14) 0.432(8) 0.193(6) 0.05(2) Uiso 1 1 d D . . . .
H4 H 0.267(10) 0.183(9) 0.191(5) 0.029(17) Uiso 1 1 d D . . . .
H8 H 1.16(3) 0.066(16) 0.624(10) 0.15(6) Uiso 1 1 d D . . . .
H9 H 1.281(18) 0.14(3) 0.561(12) 0.15(6) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ca1 O1 2.333(5) 2_766 ?
Ca1 O1 2.333(5) . ?
Ca1 O2 2.338(5) 2_666 ?
Ca1 O2 2.338(5) 1_655 ?
Ca1 O3 2.380(8) 2_766 ?
Ca1 O3 2.380(8) . ?
Ca1 H9 2.77(15) . ?
O1 C1 1.260(9) . ?
O2 C1 1.237(8) . ?
O2 Ca1 2.338(5) 1_455 ?
C1 C2 1.510(10) . ?
C2 N1 1.463(9) . ?
C2 H1 0.9700 . ?
C2 H2 0.9700 . ?
N1 C3 1.486(10) . ?
N1 H3 0.98(2) . ?
N1 H4 0.98(2) . ?
C3 H5 0.9600 . ?
C3 H7 0.9600 . ?
C3 H6 0.9600 . ?
O3 H8 0.98(2) . ?
O3 H9 0.98(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ca1 O1 180.0 2_766 . ?
O1 Ca1 O2 86.52(19) 2_766 2_666 ?
O1 Ca1 O2 93.48(19) . 2_666 ?
O1 Ca1 O2 93.5(2) 2_766 1_655 ?
O1 Ca1 O2 86.52(19) . 1_655 ?
O2 Ca1 O2 180.0 2_666 1_655 ?
O1 Ca1 O3 88.5(3) 2_766 2_766 ?
O1 Ca1 O3 91.5(3) . 2_766 ?
O2 Ca1 O3 92.0(2) 2_666 2_766 ?
O2 Ca1 O3 88.0(2) 1_655 2_766 ?
O1 Ca1 O3 91.5(3) 2_766 . ?
O1 Ca1 O3 88.5(3) . . ?
O2 Ca1 O3 88.0(2) 2_666 . ?
O2 Ca1 O3 92.0(2) 1_655 . ?
O3 Ca1 O3 180.0(4) 2_766 . ?
O1 Ca1 H9 84(3) 2_766 . ?
O1 Ca1 H9 96(3) . . ?
O2 Ca1 H9 106(2) 2_666 . ?
O2 Ca1 H9 74(2) 1_655 . ?
O3 Ca1 H9 160(2) 2_766 . ?
O3 Ca1 H9 20(2) . . ?
C1 O1 Ca1 131.2(5) . . ?
C1 O2 Ca1 129.4(5) . 1_455 ?
O2 C1 O1 126.5(7) . . ?
O2 C1 C2 117.9(6) . . ?
O1 C1 C2 115.6(6) . . ?
N1 C2 C1 113.0(6) . . ?
N1 C2 H1 109.0 . . ?
C1 C2 H1 109.0 . . ?
N1 C2 H2 109.0 . . ?
C1 C2 H2 109.0 . . ?
H1 C2 H2 107.8 . . ?
C2 N1 C3 114.6(6) . . ?
C2 N1 H3 110(5) . . ?
C3 N1 H3 109(5) . . ?
C2 N1 H4 109(4) . . ?
C3 N1 H4 113(4) . . ?
H3 N1 H4 101(6) . . ?
N1 C3 H5 109.5 . . ?
N1 C3 H7 109.5 . . ?
H5 C3 H7 109.5 . . ?
N1 C3 H6 109.5 . . ?
H5 C3 H6 109.5 . . ?
H7 C3 H6 109.5 . . ?
Ca1 O3 H8 176(9) . . ?
Ca1 O3 H9 103(10) . . ?
H8 O3 H9 75(10) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H3 I1 0.98(2) 2.56(3) 3.499(6) 162(7) .
N1 H4 I1 0.98(2) 2.59(4) 3.481(6) 151(5) 1_545

_refine_diff_density_max         1.174
_refine_diff_density_min         -0.843
_refine_diff_density_rms         0.146

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC6
_database_code_depnum_ccdc_archive 'CCDC 1841215'
_audit_update_record             
;
2018-05-03 deposited with the CCDC.
2018-06-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C9 H25 Mn N3 O8, 2(I)'
_chemical_formula_sum            'C9 H25 I2 Mn N3 O8'
_chemical_formula_weight         612.06

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   9.8652(7)
_cell_length_b                   19.2670(15)
_cell_length_c                   10.3186(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1961.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    857
_cell_measurement_theta_min      1.1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.073
_exptl_crystal_F_000             1180
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    3.858
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.739
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
'The program SADABS-2008/1 - G.M. Sheldrick was used to apply a multi-scan absorption correction.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Tube'
_diffrn_measurement_device_type  'Rigaku Mercury2 (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 13.6612
_diffrn_reflns_number            19214
_diffrn_reflns_av_unetI/netI     0.0436
_diffrn_reflns_av_R_equivalents  0.0978
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.114
_diffrn_reflns_theta_max         27.520
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2323
_reflns_number_gt                1419
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0585P)²+7.7627P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2323
_refine_ls_number_parameters     147
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0916
_refine_ls_R_factor_gt           0.0421
_refine_ls_wR_factor_ref         0.1239
_refine_ls_wR_factor_gt          0.0964
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_restrained_S_all      0.976
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.01696(5) 0.40818(2) 0.74773(5) 0.04127(18) Uani 1 1 d . . . . .
Mn2 Mn 0.40838(13) 0.7500 0.78568(12) 0.0220(3) Uani 1 2 d S T P . .
O5 O 0.5198(4) 0.6681(2) 0.6802(4) 0.0298(10) Uani 1 1 d D . . . .
O2 O 0.0454(6) 0.7500 0.5463(6) 0.0310(15) Uani 1 2 d S T P . .
O3 O 0.2967(4) 0.6640(2) 0.8775(4) 0.0262(9) Uani 1 1 d . . . . .
O1 O 0.2435(6) 0.7500 0.6493(6) 0.0377(16) Uani 1 2 d S T P . .
C4 C 0.3422(6) 0.6046(3) 0.9036(6) 0.0263(14) Uani 1 1 d . . . . .
C1 C 0.1727(9) 0.7500 0.5492(9) 0.0245(19) Uani 1 2 d S T P . .
C2 C 0.2447(9) 0.7500 0.4213(9) 0.030(2) Uani 1 2 d S T P . .
N1 N 0.1496(8) 0.7500 0.3109(8) 0.0320(18) Uani 1 2 d DS T P . .
O4 O 0.4578(4) 0.5823(2) 0.8792(5) 0.0356(11) Uani 1 1 d . . . . .
C5 C 0.2433(6) 0.5550(3) 0.9680(6) 0.0277(14) Uani 1 1 d . . . . .
H5 H 0.2027 0.5777 1.0425 0.033 Uiso 1 1 calc R U . . .
H6 H 0.1713 0.5437 0.9076 0.033 Uiso 1 1 calc R U . . .
N2 N 0.3105(6) 0.4905(3) 1.0104(5) 0.0276(12) Uani 1 1 d D . . . .
C6 C 0.2185(7) 0.4408(4) 1.0766(7) 0.0373(17) Uani 1 1 d . . . . .
H9 H 0.1773 0.4630 1.1499 0.056 Uiso 1 1 calc R U . . .
H11 H 0.2695 0.4012 1.1052 0.056 Uiso 1 1 calc R U . . .
H10 H 0.1492 0.4260 1.0174 0.056 Uiso 1 1 calc R U . . .
C3 C 0.2142(15) 0.7500 0.1808(11) 0.043(3) Uani 1 2 d S T P . .
H1 H 0.299(9) 0.714(4) 0.417(8) 0.06(3) Uiso 1 1 d . . . . .
H2 H 0.088(8) 0.711(3) 0.304(9) 0.09(3) Uiso 1 1 d D . . . .
H3 H 0.269(9) 0.712(5) 0.175(9) 0.07(3) Uiso 1 1 d . . . . .
H4 H 0.152(13) 0.7500 0.126(12) 0.05(4) Uiso 1 2 d S . P . .
H7 H 0.376(5) 0.499(3) 1.077(4) 0.020(16) Uiso 1 1 d D . . . .
H8 H 0.358(6) 0.469(3) 0.940(5) 0.036(19) Uiso 1 1 d D . . . .
H12 H 0.519(16) 0.637(7) 0.755(10) 0.19(8) Uiso 1 1 d D . . . .
H13 H 0.610(3) 0.673(3) 0.646(6) 0.033(18) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn2 O1 2.151(6) . ?
Mn2 O2 2.199(6) 6_657 ?
Mn2 O3 2.203(4) . ?
Mn2 O3 2.203(4) 8_575 ?
Mn2 O5 2.209(5) 8_575 ?
Mn2 O5 2.209(5) . ?
O2 C1 1.257(10) . ?
O2 Mn2 2.198(6) 6_557 ?
O3 C4 1.260(7) . ?
O1 C1 1.246(11) . ?
C4 O4 1.244(7) . ?
C4 C5 1.518(9) . ?
C1 C2 1.499(13) . ?
C2 N1 1.476(12) . ?
N1 C3 1.486(13) . ?
C5 N2 1.476(8) . ?
N2 C6 1.486(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Mn2 O2 168.8(2) . 6_657 ?
O1 Mn2 O3 84.43(17) . . ?
O2 Mn2 O3 88.18(16) 6_657 . ?
O1 Mn2 O3 84.43(17) . 8_575 ?
O2 Mn2 O3 88.18(16) 6_657 8_575 ?
O3 Mn2 O3 97.5(2) . 8_575 ?
O1 Mn2 O5 93.09(18) . 8_575 ?
O2 Mn2 O5 94.76(17) 6_657 8_575 ?
O3 Mn2 O5 175.79(18) . 8_575 ?
O3 Mn2 O5 85.64(16) 8_575 8_575 ?
O1 Mn2 O5 93.09(18) . . ?
O2 Mn2 O5 94.76(17) 6_657 . ?
O3 Mn2 O5 85.64(16) . . ?
O3 Mn2 O5 175.79(18) 8_575 . ?
O5 Mn2 O5 91.1(2) 8_575 . ?
C1 O2 Mn2 126.5(6) . 6_557 ?
C4 O3 Mn2 126.7(4) . . ?
C1 O1 Mn2 164.9(6) . . ?
O4 C4 O3 126.6(6) . . ?
O4 C4 C5 117.4(6) . . ?
O3 C4 C5 115.9(5) . . ?
O1 C1 O2 125.5(9) . . ?
O1 C1 C2 117.7(8) . . ?
O2 C1 C2 116.9(8) . . ?
N1 C2 C1 112.3(7) . . ?
C2 N1 C3 115.2(8) . . ?
N2 C5 C4 111.8(5) . . ?
C5 N2 C6 113.9(5) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H2 I1 0.97(2) 2.58(3) 3.515(4) 164(8) 5_566
N2 H7 I1 0.96(2) 2.72(4) 3.565(6) 147(5) 2_565
N2 H8 I1 0.96(2) 2.75(2) 3.709(5) 174(5) 6_657

_refine_diff_density_max         1.345
_refine_diff_density_min         -1.064
_refine_diff_density_rms         0.159

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC7
_database_code_depnum_ccdc_archive 'CCDC 1841211'
_audit_update_record             
;
2018-05-03 deposited with the CCDC.
2018-06-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H28 Ca N4 O8, 2(I), 2(H2O)'
_chemical_formula_sum            'C12 H32 Ca I2 N4 O10'
_chemical_formula_weight         686.29

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   11.3056(7)
_cell_length_b                   10.0982(7)
_cell_length_c                   23.1494(16)
_cell_angle_alpha                90
_cell_angle_beta                 103.484(8)
_cell_angle_gamma                90
_cell_volume                     2570.0(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    890
_cell_measurement_theta_min      1.8
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.774
_exptl_crystal_F_000             1352
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    2.694
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.428
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
'The program SADABS-2008/1 - G.M. Sheldrick was used to apply a multi-scan absorption correction.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Tube'
_diffrn_measurement_device_type  'Rigaku Mercury2 (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 13.6612
_diffrn_reflns_number            25644
_diffrn_reflns_av_unetI/netI     0.1099
_diffrn_reflns_av_R_equivalents  0.1416
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.809
_diffrn_reflns_theta_max         27.516
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5878
_reflns_number_gt                2798
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5878
_refine_ls_number_parameters     393
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.1344
_refine_ls_R_factor_gt           0.0545
_refine_ls_wR_factor_ref         0.1725
_refine_ls_wR_factor_gt          0.1360
_refine_ls_goodness_of_fit_ref   0.826
_refine_ls_restrained_S_all      0.826
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.27492(6) 0.49113(6) 0.72585(3) 0.0565(2) Uani 1 1 d . . . . .
I2 I 0.78398(7) 0.92934(7) 0.76183(3) 0.0625(2) Uani 1 1 d . . . . .
Ca1 Ca 0.5000 0.5000 0.5000 0.0288(4) Uani 1 2 d S . P . .
Ca2 Ca 0.5000 1.0000 0.5000 0.0287(4) Uani 1 2 d S . P . .
O1 O 0.3568(5) 0.4597(5) 0.5554(2) 0.0435(13) Uani 1 1 d . . . . .
O2 O 0.5562(5) 0.6810(5) 0.5598(2) 0.0373(12) Uani 1 1 d . . . . .
O3 O 0.3488(5) 0.6311(5) 0.4352(2) 0.0456(14) Uani 1 1 d . . . . .
O4 O 0.6396(5) 1.0769(6) 0.4496(2) 0.0476(14) Uani 1 1 d . . . . .
O5 O 0.6546(5) 0.8738(5) 0.5653(2) 0.0424(13) Uani 1 1 d . . . . .
O6 O 0.4500(5) 0.8200(5) 0.4358(2) 0.0401(13) Uani 1 1 d . . . . .
O7 O 0.1619(6) 0.4095(8) 0.5239(3) 0.080(2) Uani 1 1 d . . . . .
O8 O 0.8296(5) 1.0304(7) 0.4491(3) 0.0614(18) Uani 1 1 d . . . . .
O9 O 0.0751(7) 0.6325(9) 0.4638(4) 0.095(3) Uani 1 1 d D . . . .
O10 O 0.9359(7) 0.9281(9) 0.5590(4) 0.079(3) Uani 1 1 d . . . . .
N1 N 0.4004(7) 0.2739(7) 0.6376(4) 0.0442(18) Uani 1 1 d . . . . .
N2 N 0.8590(6) 0.7745(7) 0.6370(3) 0.0381(15) Uani 1 1 d . . . . .
N3 N 0.6245(7) 1.2844(8) 0.3739(3) 0.0415(18) Uani 1 1 d . . . . .
N4 N 0.1409(6) 0.7294(7) 0.3683(3) 0.0418(16) Uani 1 1 d D . . . .
C1 C 0.2654(9) 0.3933(9) 0.5555(4) 0.048(2) Uani 1 1 d . . . . .
C2 C 0.2803(10) 0.2730(11) 0.5963(5) 0.052(2) Uani 1 1 d . . . . .
C3 C 0.4315(17) 0.1555(12) 0.6746(5) 0.072(3) Uani 1 1 d . . . . .
C4 C 0.6482(6) 0.7534(7) 0.5761(3) 0.0292(15) Uani 1 1 d . . . . .
C5 C 0.7601(8) 0.6837(8) 0.6104(4) 0.0364(18) Uani 1 1 d . . . . .
C6 C 0.9739(10) 0.7036(13) 0.6644(5) 0.057(3) Uani 1 1 d . . . . .
C7 C 0.7365(7) 1.0971(8) 0.4349(3) 0.0397(19) Uani 1 1 d . . . . .
C8 C 0.7428(9) 1.2173(10) 0.3959(5) 0.050(2) Uani 1 1 d . . . . .
C9 C 0.5404(12) 1.2138(14) 0.3253(5) 0.063(3) Uani 1 1 d . . . . .
C10 C 0.3559(7) 0.7498(7) 0.4240(3) 0.0305(16) Uani 1 1 d . . . . .
C11 C 0.2412(8) 0.8204(8) 0.3908(4) 0.0384(19) Uani 1 1 d . . . . .
C12 C 0.0293(9) 0.7974(11) 0.3353(5) 0.055(2) Uani 1 1 d . . . . .
H1 H 0.279(9) 0.197(10) 0.576(4) 0.07(3) Uiso 1 1 d . . . . .
H2 H 0.234(9) 0.270(10) 0.616(4) 0.06(3) Uiso 1 1 d . . . . .
H3 H 0.449(11) 0.306(12) 0.621(5) 0.10(4) Uiso 1 1 d . . . . .
H4 H 0.395(8) 0.346(9) 0.661(4) 0.05(3) Uiso 1 1 d . . . . .
H5 H 0.444(16) 0.095(18) 0.640(8) 0.18(7) Uiso 1 1 d . . . . .
H6 H 0.380(14) 0.158(15) 0.693(7) 0.13(7) Uiso 1 1 d . . . . .
H7 H 0.511(11) 0.148(12) 0.699(5) 0.09(4) Uiso 1 1 d . . . . .
H8 H 0.797(6) 0.639(7) 0.582(3) 0.03(2) Uiso 1 1 d . . . . .
H9 H 0.739(6) 0.634(7) 0.633(3) 0.018(18) Uiso 1 1 d . . . . .
H10 H 0.881(8) 0.831(9) 0.603(4) 0.07(3) Uiso 1 1 d . . . . .
H11 H 0.841(8) 0.843(9) 0.659(4) 0.06(3) Uiso 1 1 d . . . . .
H12 H 0.995(8) 0.648(10) 0.632(4) 0.06(3) Uiso 1 1 d . . . . .
H13 H 0.951(7) 0.639(9) 0.689(4) 0.05(2) Uiso 1 1 d . . . . .
H14 H 1.028(9) 0.745(10) 0.686(4) 0.06(3) Uiso 1 1 d . . . . .
H15 H 0.808(10) 1.279(12) 0.425(5) 0.10(4) Uiso 1 1 d . . . . .
H16 H 0.761(11) 1.200(12) 0.367(5) 0.09(4) Uiso 1 1 d . . . . .
H17 H 0.593(8) 1.292(9) 0.408(4) 0.06(3) Uiso 1 1 d . . . . .
H18 H 0.646(8) 1.347(9) 0.363(4) 0.04(3) Uiso 1 1 d . . . . .
H19 H 0.520(8) 1.149(9) 0.347(4) 0.05(3) Uiso 1 1 d . . . . .
H20 H 0.586(9) 1.199(9) 0.300(4) 0.06(3) Uiso 1 1 d . . . . .
H21 H 0.485(10) 1.286(11) 0.315(5) 0.08(3) Uiso 1 1 d . . . . .
H22 H 0.214(10) 0.862(11) 0.415(5) 0.08(4) Uiso 1 1 d . . . . .
H23 H 0.256(7) 0.849(8) 0.358(4) 0.04(2) Uiso 1 1 d . . . . .
H24 H 0.127(9) 0.688(10) 0.405(3) 0.09(4) Uiso 1 1 d D . . . .
H25 H 0.169(5) 0.656(4) 0.349(2) 0.012(15) Uiso 1 1 d D . . . .
H26 H 0.017(9) 0.873(11) 0.371(5) 0.08(3) Uiso 1 1 d . . . . .
H27 H 0.048(8) 0.855(10) 0.304(4) 0.07(3) Uiso 1 1 d . . . . .
H28 H -0.037(8) 0.737(9) 0.324(4) 0.05(3) Uiso 1 1 d . . . . .
H29 H -0.005(3) 0.651(7) 0.470(3) 0.033(19) Uiso 1 1 d D . . . .
H30 H 0.113(7) 0.567(6) 0.493(3) 0.05(2) Uiso 1 1 d D . . . .
H32 H 1.014(8) 0.951(8) 0.556(3) 0.04(2) Uiso 1 1 d . . . . .
H31 H 0.891(8) 0.943(9) 0.526(4) 0.05(3) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ca1 O2 2.292(5) . ?
Ca1 O2 2.292(5) 3_666 ?
Ca1 O1 2.323(5) . ?
Ca1 O1 2.323(5) 3_666 ?
Ca1 O3 2.394(5) 3_666 ?
Ca1 O3 2.394(5) . ?
Ca2 O4 2.306(5) 3_676 ?
Ca2 O4 2.306(5) . ?
Ca2 O6 2.333(5) 3_676 ?
Ca2 O6 2.333(5) . ?
Ca2 O5 2.393(5) . ?
Ca2 O5 2.393(5) 3_676 ?
O1 C1 1.232(10) . ?
O2 C4 1.255(8) . ?
O3 C10 1.233(9) . ?
O4 C7 1.237(9) . ?
O5 C4 1.247(8) . ?
O6 C10 1.255(8) . ?
O7 C1 1.238(11) . ?
O8 C7 1.228(10) . ?
O9 H29 0.97(2) . ?
O9 H30 0.98(2) . ?
O10 H32 0.93(9) . ?
O10 H31 0.82(10) . ?
N1 C3 1.465(13) . ?
N1 C2 1.466(12) . ?
N1 H3 0.81(13) . ?
N1 H4 0.92(9) . ?
N2 C5 1.466(10) . ?
N2 C6 1.490(12) . ?
N2 H10 1.04(10) . ?
N2 H11 0.90(10) . ?
N3 C9 1.477(13) . ?
N3 C8 1.479(12) . ?
N3 H17 0.95(9) . ?
N3 H18 0.74(9) . ?
N4 C11 1.458(10) . ?
N4 C12 1.483(11) . ?
N4 H24 0.98(2) . ?
N4 H25 0.96(2) . ?
C1 C2 1.525(13) . ?
C2 H1 0.89(10) . ?
C2 H2 0.76(9) . ?
C3 H5 1.04(19) . ?
C3 H6 0.80(16) . ?
C3 H7 0.94(12) . ?
C4 C5 1.503(10) . ?
C5 H8 0.98(8) . ?
C5 H9 0.80(7) . ?
C6 H12 1.02(10) . ?
C6 H13 0.93(9) . ?
C6 H14 0.81(10) . ?
C7 C8 1.524(12) . ?
C8 H15 1.08(12) . ?
C8 H16 0.76(11) . ?
C9 H19 0.88(9) . ?
C9 H20 0.88(10) . ?
C9 H21 0.95(11) . ?
C10 C11 1.521(11) . ?
C11 H22 0.82(11) . ?
C11 H23 0.86(9) . ?
C12 H26 1.15(11) . ?
C12 H27 0.98(10) . ?
C12 H28 0.96(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ca1 O2 180.00(14) . 3_666 ?
O2 Ca1 O1 86.38(19) . . ?
O2 Ca1 O1 93.62(19) 3_666 . ?
O2 Ca1 O1 93.62(19) . 3_666 ?
O2 Ca1 O1 86.38(19) 3_666 3_666 ?
O1 Ca1 O1 180.0 . 3_666 ?
O2 Ca1 O3 90.31(19) . 3_666 ?
O2 Ca1 O3 89.69(19) 3_666 3_666 ?
O1 Ca1 O3 92.58(19) . 3_666 ?
O1 Ca1 O3 87.42(19) 3_666 3_666 ?
O2 Ca1 O3 89.69(18) . . ?
O2 Ca1 O3 90.31(19) 3_666 . ?
O1 Ca1 O3 87.42(19) . . ?
O1 Ca1 O3 92.58(19) 3_666 . ?
O3 Ca1 O3 180.0(2) 3_666 . ?
O4 Ca2 O4 180.0 3_676 . ?
O4 Ca2 O6 91.9(2) 3_676 3_676 ?
O4 Ca2 O6 88.1(2) . 3_676 ?
O4 Ca2 O6 88.1(2) 3_676 . ?
O4 Ca2 O6 91.9(2) . . ?
O6 Ca2 O6 180.0 3_676 . ?
O4 Ca2 O5 89.21(19) 3_676 . ?
O4 Ca2 O5 90.79(19) . . ?
O6 Ca2 O5 88.86(18) 3_676 . ?
O6 Ca2 O5 91.14(18) . . ?
O4 Ca2 O5 90.79(19) 3_676 3_676 ?
O4 Ca2 O5 89.21(19) . 3_676 ?
O6 Ca2 O5 91.13(18) 3_676 3_676 ?
O6 Ca2 O5 88.86(18) . 3_676 ?
O5 Ca2 O5 180.0 . 3_676 ?
C1 O1 Ca1 142.1(6) . . ?
C4 O2 Ca1 137.7(4) . . ?
C10 O3 Ca1 126.7(5) . . ?
C7 O4 Ca2 161.6(5) . . ?
C4 O5 Ca2 125.3(5) . . ?
C10 O6 Ca2 130.3(4) . . ?
H29 O9 H30 107(7) . . ?
H32 O10 H31 107(8) . . ?
C3 N1 C2 115.8(10) . . ?
C3 N1 H3 121(9) . . ?
C2 N1 H3 109(8) . . ?
C3 N1 H4 110(5) . . ?
C2 N1 H4 102(5) . . ?
H3 N1 H4 96(10) . . ?
C5 N2 C6 112.5(8) . . ?
C5 N2 H10 109(5) . . ?
C6 N2 H10 104(5) . . ?
C5 N2 H11 118(6) . . ?
C6 N2 H11 115(6) . . ?
H10 N2 H11 97(8) . . ?
C9 N3 C8 114.3(8) . . ?
C9 N3 H17 112(5) . . ?
C8 N3 H17 103(5) . . ?
C9 N3 H18 111(7) . . ?
C8 N3 H18 99(7) . . ?
H17 N3 H18 116(9) . . ?
C11 N4 C12 112.9(7) . . ?
C11 N4 H24 103(6) . . ?
C12 N4 H24 110(6) . . ?
C11 N4 H25 110(4) . . ?
C12 N4 H25 117(4) . . ?
H24 N4 H25 103(7) . . ?
O1 C1 O7 127.2(8) . . ?
O1 C1 C2 117.6(8) . . ?
O7 C1 C2 115.1(8) . . ?
N1 C2 C1 110.5(8) . . ?
N1 C2 H1 104(6) . . ?
C1 C2 H1 112(6) . . ?
N1 C2 H2 106(7) . . ?
C1 C2 H2 114(8) . . ?
H1 C2 H2 110(10) . . ?
N1 C3 H5 95(10) . . ?
N1 C3 H6 101(10) . . ?
H5 C3 H6 132(10) . . ?
N1 C3 H7 119(8) . . ?
H5 C3 H7 97(10) . . ?
H6 C3 H7 113(10) . . ?
O5 C4 O2 126.2(6) . . ?
O5 C4 C5 118.8(6) . . ?
O2 C4 C5 114.9(6) . . ?
N2 C5 C4 113.2(6) . . ?
N2 C5 H8 100(4) . . ?
C4 C5 H8 108(4) . . ?
N2 C5 H9 115(5) . . ?
C4 C5 H9 107(5) . . ?
H8 C5 H9 113(7) . . ?
N2 C6 H12 106(5) . . ?
N2 C6 H13 105(5) . . ?
H12 C6 H13 102(8) . . ?
N2 C6 H14 118(7) . . ?
H12 C6 H14 119(9) . . ?
H13 C6 H14 105(8) . . ?
O8 C7 O4 126.5(8) . . ?
O8 C7 C8 116.1(7) . . ?
O4 C7 C8 117.4(8) . . ?
N3 C8 C7 113.9(7) . . ?
N3 C8 H15 113(6) . . ?
C7 C8 H15 102(6) . . ?
N3 C8 H16 103(9) . . ?
C7 C8 H16 113(9) . . ?
H15 C8 H16 113(10) . . ?
N3 C9 H19 98(6) . . ?
N3 C9 H20 103(6) . . ?
H19 C9 H20 122(9) . . ?
N3 C9 H21 95(6) . . ?
H19 C9 H21 117(9) . . ?
H20 C9 H21 115(9) . . ?
O3 C10 O6 126.6(7) . . ?
O3 C10 C11 118.2(7) . . ?
O6 C10 C11 115.2(6) . . ?
N4 C11 C10 112.6(7) . . ?
N4 C11 H22 100(8) . . ?
C10 C11 H22 108(8) . . ?
N4 C11 H23 101(5) . . ?
C10 C11 H23 107(6) . . ?
H22 C11 H23 128(9) . . ?
N4 C12 H26 100(5) . . ?
N4 C12 H27 110(6) . . ?
H26 C12 H27 102(8) . . ?
N4 C12 H28 111(5) . . ?
H26 C12 H28 113(7) . . ?
H27 C12 H28 118(7) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H4 I1 0.92(9) 2.69(10) 3.514(8) 151(7) .
N2 H11 I2 0.90(10) 2.76(10) 3.558(7) 148(8) .
N3 H18 I1 0.74(9) 2.92(9) 3.604(8) 154(8) 3_676
N4 H25 I2 0.96(2) 2.77(4) 3.621(7) 148(5) 4_575

_refine_diff_density_max         1.015
_refine_diff_density_min         -0.815
_refine_diff_density_rms         0.162

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC8
_database_code_depnum_ccdc_archive 'CCDC 1841203'
_audit_update_record             
;
2018-05-03 deposited with the CCDC.
2018-06-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H18 Mg N2 O6, 2(Cl)'
_chemical_formula_sum            'C6 H18 Cl2 Mg N2 O6'
_chemical_formula_weight         309.43

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   4.7711(4)
_cell_length_b                   5.3186(4)
_cell_length_c                   13.5193(12)
_cell_angle_alpha                84.365(12)
_cell_angle_beta                 82.080(12)
_cell_angle_gamma                87.969(12)
_cell_volume                     338.06(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    837
_cell_measurement_theta_min      1.5
_cell_measurement_theta_max      27.5

_exptl_crystal_description       platelet
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_F_000             162
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    0.543
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.783
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
'The program SADABS-2008/1 - G.M. Sheldrick was used to apply a multi-scan absorption correction.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Tube'
_diffrn_measurement_device_type  'Rigaku Mercury2 (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 13.6612
_diffrn_reflns_number            3423
_diffrn_reflns_av_unetI/netI     0.0650
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.528
_diffrn_reflns_theta_max         27.526
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             1536
_reflns_number_gt                1094
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1536
_refine_ls_number_parameters     96
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0920
_refine_ls_R_factor_gt           0.0625
_refine_ls_wR_factor_ref         0.2468
_refine_ls_wR_factor_gt          0.2379
_refine_ls_goodness_of_fit_ref   1.639
_refine_ls_restrained_S_all      1.637
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mg1 Mg 0.0000 0.5000 0.5000 0.0157(6) Uani 1 2 d S . P . .
Cl1 Cl 0.1980(3) 0.2239(2) 0.17855(11) 0.0243(5) Uani 1 1 d . . . . .
O2 O 0.6735(8) 0.7256(7) 0.4456(3) 0.0186(9) Uani 1 1 d . . . . .
O1 O 0.2818(8) 0.6487(7) 0.3806(3) 0.0183(9) Uani 1 1 d . . . . .
O3 O -0.0707(9) 0.2176(7) 0.4116(3) 0.0228(9) Uani 1 1 d D . . . .
N1 N 0.5270(10) 0.7156(8) 0.1898(3) 0.0172(10) Uani 1 1 d D . . . .
C1 C 0.5398(11) 0.6979(9) 0.3748(4) 0.0157(11) Uani 1 1 d . . . . .
C2 C 0.7069(11) 0.7255(11) 0.2712(4) 0.0205(12) Uani 1 1 d . . . . .
H2A H 0.8033 0.8853 0.2617 0.025 Uiso 1 1 calc R U . . .
H2B H 0.8500 0.5914 0.2661 0.025 Uiso 1 1 calc R U . . .
C3 C 0.6942(14) 0.7320(12) 0.0883(4) 0.0292(14) Uani 1 1 d . . . . .
H3A H 0.8167 0.8740 0.0806 0.044 Uiso 1 1 calc R U . . .
H3B H 0.5682 0.7528 0.0384 0.044 Uiso 1 1 calc R U . . .
H3C H 0.8060 0.5798 0.0805 0.044 Uiso 1 1 calc R U . . .
H3 H 0.442(16) 0.549(8) 0.210(6) 0.05(2) Uiso 1 1 d D . . . .
H4 H 0.372(11) 0.840(11) 0.189(6) 0.05(2) Uiso 1 1 d D . . . .
H8 H 0.018(13) 0.200(12) 0.343(2) 0.030(18) Uiso 1 1 d D . . . .
H9 H -0.13(3) 0.050(11) 0.440(9) 0.12(4) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mg1 O1 2.066(4) . ?
Mg1 O1 2.066(4) 2_566 ?
Mg1 O3 2.073(4) . ?
Mg1 O3 2.073(4) 2_566 ?
Mg1 O2 2.102(4) 2_666 ?
Mg1 O2 2.102(4) 1_455 ?
O2 C1 1.244(6) . ?
O2 Mg1 2.102(4) 1_655 ?
O1 C1 1.257(6) . ?
O3 H8 0.97(2) . ?
O3 H9 0.97(2) . ?
N1 C3 1.485(7) . ?
N1 C2 1.492(7) . ?
N1 H3 0.98(2) . ?
N1 H4 0.98(2) . ?
C1 C2 1.510(7) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Mg1 O1 180.0 . 2_566 ?
O1 Mg1 O3 87.23(14) . . ?
O1 Mg1 O3 92.77(15) 2_566 . ?
O1 Mg1 O3 92.77(15) . 2_566 ?
O1 Mg1 O3 87.23(15) 2_566 2_566 ?
O3 Mg1 O3 180.0 . 2_566 ?
O1 Mg1 O2 90.24(14) . 2_666 ?
O1 Mg1 O2 89.76(14) 2_566 2_666 ?
O3 Mg1 O2 89.08(15) . 2_666 ?
O3 Mg1 O2 90.92(15) 2_566 2_666 ?
O1 Mg1 O2 89.76(14) . 1_455 ?
O1 Mg1 O2 90.24(14) 2_566 1_455 ?
O3 Mg1 O2 90.92(15) . 1_455 ?
O3 Mg1 O2 89.08(15) 2_566 1_455 ?
O2 Mg1 O2 180.00(19) 2_666 1_455 ?
C1 O2 Mg1 129.7(3) . 1_655 ?
C1 O1 Mg1 130.8(3) . . ?
Mg1 O3 H8 127(4) . . ?
Mg1 O3 H9 122(8) . . ?
H8 O3 H9 107(9) . . ?
C3 N1 C2 112.7(5) . . ?
C3 N1 H3 113(5) . . ?
C2 N1 H3 100(5) . . ?
C3 N1 H4 108(5) . . ?
C2 N1 H4 116(5) . . ?
H3 N1 H4 107(6) . . ?
O2 C1 O1 126.9(5) . . ?
O2 C1 C2 116.1(5) . . ?
O1 C1 C2 116.9(5) . . ?
N1 C2 C1 113.0(4) . . ?
N1 C2 H2A 109.0 . . ?
C1 C2 H2A 109.0 . . ?
N1 C2 H2B 109.0 . . ?
C1 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
N1 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H3 Cl1 0.98(2) 2.23(4) 3.124(4) 151(7) .
N1 H4 Cl1 0.98(2) 2.17(4) 3.079(5) 154(7) 1_565

_refine_diff_density_max         0.688
_refine_diff_density_min         -0.408
_refine_diff_density_rms         0.119

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC9
_database_code_depnum_ccdc_archive 'CCDC 1841216'
_audit_update_record             
;
2018-05-03 deposited with the CCDC.
2018-06-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C9 H21 N3 O6 Sr, 2(Br)'
_chemical_formula_sum            'C9 H21 Br2 N3 O6 Sr'
_chemical_formula_weight         514.73

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Sr Sr -1.5307 3.2498 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      Orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P cab'
_space_group_name_Hall           '-P 2bc 2ac'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y+1/2, z+1/2'
'x+1/2, -y, -z+1/2'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'-x-1/2, y, z-1/2'
'x-1/2, -y-1/2, z'

_cell_length_a                   8.7723(6)
_cell_length_b                   10.5359(7)
_cell_length_c                   36.5820(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3381.1(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    900
_cell_measurement_theta_min      1.7
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.022
_exptl_crystal_F_000             2016
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    7.943
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.723
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
'The program SADABS-2008/1 - G.M. Sheldrick was used to apply a multi-scan absorption correction.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Tube'
_diffrn_measurement_device_type  'Rigaku Mercury2 (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 13.6612
_diffrn_reflns_number            31461
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_theta_min         2.227
_diffrn_reflns_theta_max         27.509
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             3873
_reflns_number_gt                3172
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3873
_refine_ls_number_parameters     274
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0307
_refine_ls_wR_factor_ref         0.1299
_refine_ls_wR_factor_gt          0.1102
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.015
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sr2 Sr 0.04895(4) -0.25922(3) 0.62493(2) 0.01240(14) Uani 1 1 d . . . . .
Br1A Br 0.00751(4) 0.27938(4) 0.54406(2) 0.02307(15) Uani 1 1 d . . . . .
Br1B Br 0.04057(5) 0.24716(3) 0.70941(2) 0.02140(15) Uani 1 1 d . . . . .
O1 O 0.2545(4) -0.0949(3) 0.61603(7) 0.0381(7) Uani 1 1 d . . . . .
O2 O 0.4677(3) -0.0074(2) 0.63658(8) 0.0311(6) Uani 1 1 d . . . . .
C1 C 0.3323(5) -0.0029(3) 0.62585(9) 0.0247(8) Uani 1 1 d . . . . .
C2 C 0.2553(4) 0.1268(3) 0.62441(9) 0.0203(7) Uani 1 1 d . . . . .
N1 N 0.3697(4) 0.2305(3) 0.62760(9) 0.0177(6) Uani 1 1 d . . . . .
C3 C 0.3037(5) 0.3594(4) 0.62668(11) 0.0278(9) Uani 1 1 d . . . . .
O3A O -0.1102(4) -0.1397(3) 0.58247(8) 0.0480(9) Uani 1 1 d . . . . .
O4A O -0.3545(3) -0.1381(3) 0.56549(7) 0.0328(7) Uani 1 1 d . . . . .
C4A C -0.2173(5) -0.1145(3) 0.56123(9) 0.0220(8) Uani 1 1 d . . . . .
C5A C -0.1684(4) -0.0477(3) 0.52633(9) 0.0186(7) Uani 1 1 d . . . . .
N2A N -0.2999(3) -0.0085(3) 0.50387(8) 0.0177(6) Uani 1 1 d . . . . .
C6A C -0.2579(5) 0.0658(4) 0.47098(10) 0.0298(9) Uani 1 1 d . . . . .
O3B O 0.2769(3) -0.3236(3) 0.66246(7) 0.0337(7) Uani 1 1 d . . . . .
O4B O 0.4992(3) -0.3715(4) 0.68600(8) 0.0459(9) Uani 1 1 d . . . . .
C4B C 0.3582(4) -0.3723(3) 0.68638(9) 0.0213(7) Uani 1 1 d . . . . .
C5B C 0.2767(4) -0.4365(3) 0.71814(9) 0.0175(7) Uani 1 1 d . . . . .
N2B N 0.3874(4) -0.4876(3) 0.74489(8) 0.0204(6) Uani 1 1 d . . . . .
C6B C 0.3152(5) -0.5531(4) 0.77650(10) 0.0296(9) Uani 1 1 d . . . . .
H1A H 0.197(4) 0.144(3) 0.6010(10) 0.014(9) Uiso 1 1 d . . . . .
H1B H 0.192(4) 0.135(4) 0.6442(11) 0.023(11) Uiso 1 1 d . . . . .
H2A H 0.447(4) 0.228(3) 0.6099(10) 0.009(9) Uiso 1 1 d . . . . .
H2B H 0.411(5) 0.229(4) 0.6461(13) 0.023(12) Uiso 1 1 d . . . . .
H3A H 0.242(5) 0.365(4) 0.6054(12) 0.033(12) Uiso 1 1 d . . . . .
H3B H 0.236(5) 0.365(3) 0.6470(11) 0.019(10) Uiso 1 1 d . . . . .
H4 H 0.394(6) 0.416(6) 0.6300(13) 0.058(16) Uiso 1 1 d . . . . .
H5A H -0.118(4) 0.026(4) 0.5305(9) 0.010(8) Uiso 1 1 d . . . . .
H6A H -0.104(4) -0.103(3) 0.5121(9) 0.013(9) Uiso 1 1 d . . . . .
H7A H -0.358(5) 0.041(4) 0.5176(10) 0.020(10) Uiso 1 1 d . . . . .
H8A H -0.355(6) -0.071(5) 0.4962(13) 0.049(14) Uiso 1 1 d . . . . .
H9A H -0.196(4) 0.147(4) 0.4766(11) 0.020(10) Uiso 1 1 d . . . . .
H10A H -0.185(5) 0.015(4) 0.4561(12) 0.032(12) Uiso 1 1 d . . . . .
H11A H -0.355(5) 0.099(4) 0.4576(12) 0.034(12) Uiso 1 1 d . . . . .
H5B H 0.210(4) -0.377(4) 0.7312(11) 0.022(10) Uiso 1 1 d . . . . .
H6B H 0.219(4) -0.509(3) 0.7116(9) 0.004(8) Uiso 1 1 d . . . . .
H7B H 0.441(4) -0.416(4) 0.7531(11) 0.029(11) Uiso 1 1 d . . . . .
H8B H 0.445(4) -0.546(4) 0.7329(10) 0.022(10) Uiso 1 1 d . . . . .
H9B H 0.254(6) -0.492(5) 0.7877(13) 0.046(14) Uiso 1 1 d . . . . .
H10B H 0.252(6) -0.626(4) 0.7696(13) 0.045(13) Uiso 1 1 d . . . . .
H11B H 0.398(4) -0.593(4) 0.7927(10) 0.018(10) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sr2 O3A 2.438(3) . ?
Sr2 O3B 2.518(3) . ?
Sr2 O1 2.521(3) . ?
Sr2 O4A 2.572(2) 8_655 ?
Sr2 O2 2.595(3) 8 ?
Sr2 O4B 2.660(3) 8 ?
Sr2 O3B 2.888(3) 8 ?
Sr2 O1 3.024(3) 8 ?
Sr2 C4B 3.126(4) 8 ?
Sr2 C1 3.146(4) 8 ?
Sr2 C4A 3.377(4) 8_655 ?
Sr2 Sr2 4.3904(3) 8 ?
O1 C1 1.239(5) . ?
O1 Sr2 3.023(3) 8_655 ?
O2 C1 1.252(5) . ?
O2 Sr2 2.595(3) 8_655 ?
C1 C2 1.525(5) . ?
C1 Sr2 3.146(4) 8_655 ?
C2 N1 1.488(5) . ?
N1 C3 1.477(5) . ?
O3A C4A 1.248(5) . ?
O4A C4A 1.239(5) . ?
O4A Sr2 2.572(2) 8 ?
C4A C5A 1.520(5) . ?
C4A Sr2 3.377(4) 8 ?
C5A N2A 1.475(4) . ?
N2A C6A 1.482(4) . ?
O3B C4B 1.241(4) . ?
O3B Sr2 2.888(3) 8_655 ?
O4B C4B 1.237(5) . ?
O4B Sr2 2.660(3) 8_655 ?
C4B C5B 1.522(5) . ?
C4B Sr2 3.126(4) 8_655 ?
C5B N2B 1.480(4) . ?
N2B C6B 1.488(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3A Sr2 O3B 160.18(11) . . ?
O3A Sr2 O1 88.42(11) . . ?
O3B Sr2 O1 71.80(10) . . ?
O3A Sr2 O4A 82.36(10) . 8_655 ?
O3B Sr2 O4A 94.94(10) . 8_655 ?
O1 Sr2 O4A 86.79(9) . 8_655 ?
O3A Sr2 O2 115.89(11) . 8 ?
O3B Sr2 O2 82.72(9) . 8 ?
O1 Sr2 O2 150.26(10) . 8 ?
O4A Sr2 O2 80.26(9) 8_655 8 ?
O3A Sr2 O4B 100.01(11) . 8 ?
O3B Sr2 O4B 79.16(9) . 8 ?
O1 Sr2 O4B 82.54(10) . 8 ?
O4A Sr2 O4B 168.98(10) 8_655 8 ?
O2 Sr2 O4B 107.93(10) 8 8 ?
O3A Sr2 O3B 70.96(10) . 8 ?
O3B Sr2 O3B 118.58(10) . 8 ?
O1 Sr2 O3B 116.42(9) . 8 ?
O4A Sr2 O3B 143.22(9) 8_655 8 ?
O2 Sr2 O3B 88.93(9) 8 8 ?
O4B Sr2 O3B 46.30(8) 8 8 ?
O3A Sr2 O1 72.83(10) . 8 ?
O3B Sr2 O1 126.88(8) . 8 ?
O1 Sr2 O1 161.14(10) . 8 ?
O4A Sr2 O1 88.65(9) 8_655 8 ?
O2 Sr2 O1 45.69(8) 8 8 ?
O4B Sr2 O1 102.34(8) 8 8 ?
O3B Sr2 O1 59.92(7) 8 8 ?
O3A Sr2 C4B 85.57(10) . 8 ?
O3B Sr2 C4B 98.77(9) . 8 ?
O1 Sr2 C4B 99.86(10) . 8 ?
O4A Sr2 C4B 166.06(9) 8_655 8 ?
O2 Sr2 C4B 98.93(9) 8 8 ?
O4B Sr2 C4B 22.93(9) 8 8 ?
O3B Sr2 C4B 23.37(8) 8 8 ?
O1 Sr2 C4B 81.12(8) 8 8 ?
O3A Sr2 C1 94.16(11) . 8 ?
O3B Sr2 C1 105.02(10) . 8 ?
O1 Sr2 C1 168.74(10) . 8 ?
O4A Sr2 C1 82.70(9) 8_655 8 ?
O2 Sr2 C1 22.69(9) 8 8 ?
O4B Sr2 C1 107.73(10) 8 8 ?
O3B Sr2 C1 74.72(9) 8 8 ?
O1 Sr2 C1 23.07(9) 8 8 ?
C4B Sr2 C1 91.27(9) 8 8 ?
O3A Sr2 C4A 96.40(10) . 8_655 ?
O3B Sr2 C4A 77.75(9) . 8_655 ?
O1 Sr2 C4A 75.35(9) . 8_655 ?
O4A Sr2 C4A 18.39(9) 8_655 8_655 ?
O2 Sr2 C4A 84.65(9) 8 8_655 ?
O4B Sr2 C4A 151.98(9) 8 8_655 ?
O3B Sr2 C4A 161.58(8) 8 8_655 ?
O1 Sr2 C4A 104.14(8) 8 8_655 ?
C4B Sr2 C4A 174.72(9) 8 8_655 ?
C1 Sr2 C4A 93.46(9) 8 8_655 ?
O3A Sr2 Sr2 53.51(8) . 8 ?
O3B Sr2 Sr2 143.62(7) . 8 ?
O1 Sr2 Sr2 133.17(8) . 8 ?
O4A Sr2 Sr2 110.34(7) 8_655 8 ?
O2 Sr2 Sr2 76.56(7) 8 8 ?
O4B Sr2 Sr2 79.25(6) 8 8 ?
O3B Sr2 Sr2 32.98(5) 8 8 ?
O1 Sr2 Sr2 33.79(5) 8 8 ?
C4B Sr2 Sr2 56.34(7) 8 8 ?
C1 Sr2 Sr2 55.37(7) 8 8 ?
C4A Sr2 Sr2 128.62(7) 8_655 8 ?
C1 O1 Sr2 153.4(3) . . ?
C1 O1 Sr2 84.0(3) . 8_655 ?
Sr2 O1 Sr2 104.36(9) . 8_655 ?
C1 O2 Sr2 104.2(2) . 8_655 ?
O1 C1 O2 125.7(4) . . ?
O1 C1 C2 116.5(4) . . ?
O2 C1 C2 117.7(3) . . ?
O1 C1 Sr2 72.9(2) . 8_655 ?
O2 C1 Sr2 53.11(19) . 8_655 ?
C2 C1 Sr2 168.8(3) . 8_655 ?
N1 C2 C1 110.9(3) . . ?
C3 N1 C2 114.1(3) . . ?
C4A O3A Sr2 159.6(3) . . ?
C4A O4A Sr2 120.7(2) . 8 ?
O4A C4A O3A 127.6(4) . . ?
O4A C4A C5A 118.2(3) . . ?
O3A C4A C5A 114.2(4) . . ?
O4A C4A Sr2 40.91(18) . 8 ?
O3A C4A Sr2 86.8(2) . 8 ?
C5A C4A Sr2 159.0(3) . 8 ?
N2A C5A C4A 112.2(3) . . ?
C5A N2A C6A 114.0(3) . . ?
C4B O3B Sr2 162.3(3) . . ?
C4B O3B Sr2 89.1(2) . 8_655 ?
Sr2 O3B Sr2 108.40(9) . 8_655 ?
C4B O4B Sr2 100.2(2) . 8_655 ?
O4B C4B O3B 124.4(3) . . ?
O4B C4B C5B 118.8(3) . . ?
O3B C4B C5B 116.9(3) . . ?
O4B C4B Sr2 56.88(19) . 8_655 ?
O3B C4B Sr2 67.5(2) . 8_655 ?
C5B C4B Sr2 175.5(2) . 8_655 ?
N2B C5B C4B 111.0(3) . . ?
C5B N2B C6B 113.7(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H2A Br1A 0.93(4) 2.47(4) 3.288(3) 146(3) 8_665
N1 H2B Br1B 0.77(5) 2.59(5) 3.355(3) 173(4) 8_665
N2A H7A Br1A 0.89(4) 2.43(4) 3.293(3) 164(3) 8_565
N2A H8A Br1A 0.86(5) 2.54(5) 3.374(3) 163(4) 4_446
N2B H7B Br1B 0.94(4) 2.41(4) 3.320(3) 163(3) 3_556
N2B H8B Br1B 0.91(4) 2.43(4) 3.311(3) 162(3) 8_655

_refine_diff_density_max         0.775
_refine_diff_density_min         -1.122
_refine_diff_density_rms         0.118

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC10
_database_code_depnum_ccdc_archive 'CCDC 1841219'
_audit_update_record             
;
2018-05-03 deposited with the CCDC.
2018-06-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C9 H21 N3 O6 Sr, 2(Cl)'
_chemical_formula_sum            'C9 H21 Cl2 N3 O6 Sr'
_chemical_formula_weight         425.81

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Sr Sr -1.5307 3.2498 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      Monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/a'
_space_group_name_Hall           '-P 2yab'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x-1/2, -y-1/2, z'

_cell_length_a                   8.7930(6)
_cell_length_b                   10.3957(7)
_cell_length_c                   17.9000(13)
_cell_angle_alpha                90
_cell_angle_beta                 91.982(6)
_cell_angle_gamma                90
_cell_volume                     1635.2(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    882
_cell_measurement_theta_min      2.0
_cell_measurement_theta_max      27.5

_exptl_crystal_description       Block
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.730
_exptl_crystal_F_000             864
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    3.651
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.847
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
'The program SADABS-2008/1 - G.M. Sheldrick was used to apply a multi-scan absorption correction.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Tube'
_diffrn_measurement_device_type  'Rigaku Mercury2 (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 13.6612
_diffrn_reflns_number            16549
_diffrn_reflns_av_unetI/netI     0.0792
_diffrn_reflns_av_R_equivalents  0.1041
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.266
_diffrn_reflns_theta_max         27.508
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3758
_reflns_number_gt                2432
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3758
_refine_ls_number_parameters     274
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0955
_refine_ls_R_factor_gt           0.0451
_refine_ls_wR_factor_ref         0.1431
_refine_ls_wR_factor_gt          0.1118
_refine_ls_goodness_of_fit_ref   0.857
_refine_ls_restrained_S_all      0.857
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sr1 Sr 0.02879(6) 0.23954(4) 0.24658(2) 0.01995(16) Uani 1 1 d . . . . .
Cl1A Cl 0.49393(18) -0.28521(14) 0.41350(8) 0.0382(4) Uani 1 1 d . . . . .
Cl1B Cl 0.49369(18) -0.22206(14) 0.08383(8) 0.0366(3) Uani 1 1 d . . . . .
O1 O -0.0582(5) 0.0049(4) 0.2261(3) 0.0435(11) Uani 1 1 d . . . . .
O2 O -0.2789(6) 0.0843(5) 0.2599(3) 0.0639(16) Uani 1 1 d . . . . .
C1 C -0.1922(7) -0.0046(5) 0.2455(3) 0.0295(13) Uani 1 1 d . . . . .
C2 C -0.2614(7) -0.1389(5) 0.2494(3) 0.0287(12) Uani 1 1 d . . . . .
N1 N -0.1423(6) -0.2390(4) 0.2476(3) 0.0269(10) Uani 1 1 d . . . . .
C3 C -0.2056(11) -0.3720(6) 0.2499(5) 0.0490(19) Uani 1 1 d . . . . .
O3A O 0.1398(5) 0.1325(4) 0.3654(2) 0.0451(11) Uani 1 1 d . . . . .
O4A O 0.3837(6) 0.1510(5) 0.3408(3) 0.0597(14) Uani 1 1 d . . . . .
C4A C 0.2773(7) 0.1167(5) 0.3797(3) 0.0319(13) Uani 1 1 d . . . . .
C5A C 0.3259(6) 0.0474(5) 0.4503(3) 0.0263(12) Uani 1 1 d . . . . .
N2A N 0.1951(6) 0.0036(5) 0.4938(3) 0.0257(10) Uani 1 1 d . . . . .
C6A C 0.2405(10) -0.0732(8) 0.5597(4) 0.0474(18) Uani 1 1 d . . . . .
O3B O 0.2638(4) 0.1748(4) 0.1780(2) 0.0367(10) Uani 1 1 d . . . . .
O4B O 0.4642(5) 0.1379(5) 0.1110(2) 0.0439(11) Uani 1 1 d . . . . .
C4B C 0.3257(6) 0.1314(5) 0.1214(3) 0.0253(11) Uani 1 1 d . . . . .
C5B C 0.2205(7) 0.0693(6) 0.0633(3) 0.0289(12) Uani 1 1 d . . . . .
N2B N 0.3053(6) 0.0083(5) 0.0022(3) 0.0257(10) Uani 1 1 d . . . . .
C6B C 0.2022(9) -0.0511(7) -0.0556(4) 0.0366(15) Uani 1 1 d . . . . .
H1A H -0.313(7) -0.157(6) 0.294(4) 0.049(19) Uiso 1 1 d . . . . .
H1B H -0.329(8) -0.148(7) 0.201(4) 0.07(2) Uiso 1 1 d . . . . .
H2A H -0.073(9) -0.225(7) 0.285(4) 0.06(2) Uiso 1 1 d . . . . .
H2B H -0.097(6) -0.230(4) 0.206(3) 0.010(12) Uiso 1 1 d . . . . .
H3A H -0.250(8) -0.371(6) 0.292(4) 0.04(2) Uiso 1 1 d . . . . .
H3B H -0.295(14) -0.382(12) 0.220(7) 0.15(5) Uiso 1 1 d . . . . .
H4 H -0.116(9) -0.429(7) 0.240(4) 0.06(2) Uiso 1 1 d . . . . .
H5A H 0.379(6) -0.026(6) 0.438(3) 0.030(15) Uiso 1 1 d . . . . .
H6A H 0.386(6) 0.102(5) 0.486(3) 0.028(15) Uiso 1 1 d . . . . .
H7A H 0.127(7) -0.042(6) 0.464(3) 0.030(16) Uiso 1 1 d . . . . .
H8A H 0.147(6) 0.068(5) 0.505(3) 0.014(13) Uiso 1 1 d . . . . .
H9A H 0.286(8) -0.145(7) 0.543(4) 0.05(2) Uiso 1 1 d . . . . .
H10A H 0.298(8) -0.019(7) 0.581(4) 0.05(2) Uiso 1 1 d . . . . .
H11A H 0.144(9) -0.097(8) 0.583(4) 0.08(3) Uiso 1 1 d . . . . .
H5B H 0.158(8) -0.003(7) 0.087(4) 0.052(19) Uiso 1 1 d . . . . .
H6B H 0.153(7) 0.134(6) 0.042(3) 0.043(18) Uiso 1 1 d . . . . .
H7B H 0.364(8) -0.046(7) 0.020(4) 0.05(2) Uiso 1 1 d . . . . .
H8B H 0.366(7) 0.069(6) -0.015(3) 0.033(17) Uiso 1 1 d . . . . .
H9B H 0.147(9) -0.121(8) -0.035(4) 0.07(3) Uiso 1 1 d . . . . .
H10B H 0.135(9) 0.018(8) -0.070(4) 0.07(3) Uiso 1 1 d . . . . .
H11B H 0.253(8) -0.086(7) -0.082(4) 0.05(2) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sr1 O4A 2.433(4) 4_565 ?
Sr1 O2 2.498(4) 4_665 ?
Sr1 O3B 2.531(4) . ?
Sr1 O3A 2.564(4) . ?
Sr1 O1 2.579(4) . ?
Sr1 O3B 2.745(4) 4_565 ?
Sr1 O4B 2.782(4) 4_565 ?
Sr1 C4B 3.120(5) 4_565 ?
Sr1 O2 3.167(6) . ?
Sr1 C1 3.196(6) . ?
Sr1 Sr1 4.4019(3) 4_665 ?
Sr1 Sr1 4.4019(3) 4_565 ?
O1 C1 1.244(7) . ?
O2 C1 1.231(7) . ?
O2 Sr1 2.498(4) 4_565 ?
C1 C2 1.526(8) . ?
C2 N1 1.478(7) . ?
N1 C3 1.491(8) . ?
O3A C4A 1.238(7) . ?
O4A C4A 1.237(7) . ?
O4A Sr1 2.433(4) 4_665 ?
C4A C5A 1.504(8) . ?
C5A N2A 1.483(7) . ?
N2A C6A 1.467(8) . ?
O3B C4B 1.250(6) . ?
O3B Sr1 2.745(4) 4_665 ?
O4B C4B 1.241(6) . ?
O4B Sr1 2.782(4) 4_665 ?
C4B C5B 1.513(8) . ?
C4B Sr1 3.120(5) 4_665 ?
C5B N2B 1.486(7) . ?
N2B C6B 1.487(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4A Sr1 O2 87.72(18) 4_565 4_665 ?
O4A Sr1 O3B 156.54(16) 4_565 . ?
O2 Sr1 O3B 71.34(16) 4_665 . ?
O4A Sr1 O3A 79.71(16) 4_565 . ?
O2 Sr1 O3A 90.10(16) 4_665 . ?
O3B Sr1 O3A 89.63(14) . . ?
O4A Sr1 O1 112.40(17) 4_565 . ?
O2 Sr1 O1 154.61(18) 4_665 . ?
O3B Sr1 O1 85.57(14) . . ?
O3A Sr1 O1 79.04(14) . . ?
O4A Sr1 O3B 72.62(15) 4_565 4_565 ?
O2 Sr1 O3B 111.49(16) 4_665 4_565 ?
O3B Sr1 O3B 124.31(16) . 4_565 ?
O3A Sr1 O3B 143.63(14) . 4_565 ?
O1 Sr1 O3B 90.01(13) . 4_565 ?
O4A Sr1 O4B 107.15(15) 4_565 4_565 ?
O2 Sr1 O4B 82.23(15) 4_665 4_565 ?
O3B Sr1 O4B 81.00(13) . 4_565 ?
O3A Sr1 O4B 169.40(14) . 4_565 ?
O1 Sr1 O4B 104.98(14) . 4_565 ?
O3B Sr1 O4B 46.89(11) 4_565 4_565 ?
O4A Sr1 C4B 89.79(15) 4_565 4_565 ?
O2 Sr1 C4B 97.02(16) 4_665 4_565 ?
O3B Sr1 C4B 102.84(14) . 4_565 ?
O3A Sr1 C4B 167.08(15) . 4_565 ?
O1 Sr1 C4B 98.33(14) . 4_565 ?
O3B Sr1 C4B 23.52(12) 4_565 4_565 ?
O4B Sr1 C4B 23.38(12) 4_565 4_565 ?
O4A Sr1 O2 73.51(16) 4_565 . ?
O2 Sr1 O2 160.66(16) 4_665 . ?
O3B Sr1 O2 127.97(12) . . ?
O3A Sr1 O2 91.04(13) . . ?
O1 Sr1 O2 43.84(13) . . ?
O3B Sr1 O2 58.97(11) 4_565 . ?
O4B Sr1 O2 98.63(12) 4_565 . ?
C4B Sr1 O2 78.68(13) 4_565 . ?
O4A Sr1 C1 92.44(17) 4_565 . ?
O2 Sr1 C1 172.75(16) 4_665 . ?
O3B Sr1 C1 107.00(14) . . ?
O3A Sr1 C1 82.79(14) . . ?
O1 Sr1 C1 21.68(13) . . ?
O3B Sr1 C1 75.41(13) 4_565 . ?
O4B Sr1 C1 104.62(13) 4_565 . ?
C4B Sr1 C1 90.23(14) 4_565 . ?
O2 Sr1 C1 22.31(13) . . ?
O4A Sr1 Sr1 121.64(13) 4_565 4_665 ?
O2 Sr1 Sr1 44.86(14) 4_665 4_665 ?
O3B Sr1 Sr1 35.02(9) . 4_665 ?
O3A Sr1 Sr1 70.72(11) . 4_665 ?
O1 Sr1 Sr1 109.76(10) . 4_665 ?
O3B Sr1 Sr1 144.73(8) 4_565 4_665 ?
O4B Sr1 Sr1 98.69(8) 4_565 4_665 ?
C4B Sr1 Sr1 121.72(10) 4_565 4_665 ?
O2 Sr1 Sr1 151.79(8) . 4_665 ?
C1 Sr1 Sr1 130.27(10) . 4_665 ?
O4A Sr1 Sr1 55.20(13) 4_565 4_565 ?
O2 Sr1 Sr1 129.53(14) 4_665 4_565 ?
O3B Sr1 Sr1 147.70(9) . 4_565 ?
O3A Sr1 Sr1 111.91(11) . 4_565 ?
O1 Sr1 Sr1 75.84(10) . 4_565 ?
O3B Sr1 Sr1 31.95(8) 4_565 4_565 ?
O4B Sr1 Sr1 78.68(8) 4_565 4_565 ?
C4B Sr1 Sr1 55.38(10) 4_565 4_565 ?
O2 Sr1 Sr1 33.81(7) . 4_565 ?
C1 Sr1 Sr1 55.40(10) . 4_565 ?
Sr1 Sr1 Sr1 174.34(2) 4_665 4_565 ?
C1 O1 Sr1 108.3(3) . . ?
C1 O2 Sr1 162.2(4) . 4_565 ?
C1 O2 Sr1 80.2(4) . . ?
Sr1 O2 Sr1 101.33(17) 4_565 . ?
O2 C1 O1 126.8(6) . . ?
O2 C1 C2 115.2(6) . . ?
O1 C1 C2 117.9(5) . . ?
O2 C1 Sr1 77.5(4) . . ?
O1 C1 Sr1 50.0(3) . . ?
C2 C1 Sr1 165.9(4) . . ?
N1 C2 C1 111.1(5) . . ?
C2 N1 C3 112.8(5) . . ?
C4A O3A Sr1 124.7(4) . . ?
C4A O4A Sr1 161.7(5) . 4_665 ?
O4A C4A O3A 126.7(6) . . ?
O4A C4A C5A 114.4(6) . . ?
O3A C4A C5A 118.9(5) . . ?
N2A C5A C4A 112.7(5) . . ?
C6A N2A C5A 113.2(5) . . ?
C4B O3B Sr1 151.0(4) . . ?
C4B O3B Sr1 95.3(3) . 4_665 ?
Sr1 O3B Sr1 113.03(14) . 4_665 ?
C4B O4B Sr1 93.8(3) . 4_665 ?
O4B C4B O3B 124.0(5) . . ?
O4B C4B C5B 120.0(5) . . ?
O3B C4B C5B 116.0(5) . . ?
O4B C4B Sr1 62.8(3) . 4_665 ?
O3B C4B Sr1 61.1(3) . 4_665 ?
C5B C4B Sr1 177.1(4) . 4_665 ?
N2B C5B C4B 112.2(5) . . ?
C5B N2B C6B 112.4(5) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H2A Cl1A 0.90(8) 2.36(8) 3.174(5) 151(7) 4
N1 H2B Cl1B 0.86(5) 2.41(5) 3.229(5) 160(4) 4
N2A H7A Cl1A 0.92(6) 2.31(6) 3.189(5) 160(5) 4
N2A H8A Cl1A 0.83(5) 2.47(5) 3.245(5) 157(5) 2_556
N2B H7B Cl1B 0.82(7) 2.42(8) 3.232(5) 169(7) .
N2B H8B Cl1B 0.89(6) 2.38(6) 3.259(5) 169(5) 3_655

_refine_diff_density_max         0.819
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.113

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC11
_database_code_depnum_ccdc_archive 'CCDC 1841205'
_audit_update_record             
;
2018-05-03 deposited with the CCDC.
2018-06-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H18 Mn N2 O6, 2(Cl)'
_chemical_formula_sum            'C6 H18 Cl2 Mn N2 O6'
_chemical_formula_weight         340.06

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   4.8078(4)
_cell_length_b                   5.3548(4)
_cell_length_c                   13.6620(12)
_cell_angle_alpha                83.825(12)
_cell_angle_beta                 82.288(12)
_cell_angle_gamma                87.503(12)
_cell_volume                     346.37(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    812
_cell_measurement_theta_min      1.5
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_F_000             175
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    1.354
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.763
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
'The program SADABS-2008/1 - G.M. Sheldrick was used to apply a multi-scan absorption correction.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Tube'
_diffrn_measurement_device_type  'Rigaku Mercury2 (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 13.6612
_diffrn_reflns_number            3548
_diffrn_reflns_av_unetI/netI     0.0702
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.512
_diffrn_reflns_theta_max         27.508
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             1574
_reflns_number_gt                1064
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1574
_refine_ls_number_parameters     115
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0429
_refine_ls_wR_factor_ref         0.1289
_refine_ls_wR_factor_gt          0.1082
_refine_ls_goodness_of_fit_ref   0.815
_refine_ls_restrained_S_all      0.815
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.0000 0.5000 0.5000 0.0172(2) Uani 1 2 d S . P . .
Cl1 Cl 0.2057(2) 0.22473(16) 0.17819(7) 0.0261(3) Uani 1 1 d . . . . .
O2 O 0.6590(5) 0.7361(4) 0.44278(18) 0.0183(5) Uani 1 1 d . . . . .
O1 O 0.2828(5) 0.6491(5) 0.37393(19) 0.0215(6) Uani 1 1 d . . . . .
O3 O -0.0718(7) 0.2096(5) 0.4075(2) 0.0262(6) Uani 1 1 d . . . . .
N1 N 0.5355(7) 0.7144(6) 0.1878(2) 0.0203(7) Uani 1 1 d . . . . .
C1 C 0.5357(7) 0.7036(6) 0.3698(3) 0.0169(7) Uani 1 1 d . . . . .
C2 C 0.7079(8) 0.7289(8) 0.2682(3) 0.0211(8) Uani 1 1 d . . . . .
C3 C 0.7020(10) 0.7318(9) 0.0875(3) 0.0306(9) Uani 1 1 d . . . . .
H1 H 0.843(10) 0.603(9) 0.266(4) 0.035(12) Uiso 1 1 d . . . . .
H2 H 0.786(9) 0.904(9) 0.258(3) 0.036(12) Uiso 1 1 d . . . . .
H3 H 0.437(8) 0.569(8) 0.200(3) 0.013(9) Uiso 1 1 d . . . . .
H4 H 0.408(8) 0.857(8) 0.187(3) 0.025(11) Uiso 1 1 d . . . . .
H5 H 0.842(11) 0.588(11) 0.084(4) 0.052(15) Uiso 1 1 d . . . . .
H6 H 0.769(8) 0.892(8) 0.080(3) 0.021(11) Uiso 1 1 d . . . . .
H7 H 0.580(10) 0.706(9) 0.040(4) 0.042(14) Uiso 1 1 d . . . . .
H8 H 0.024(11) 0.195(10) 0.354(4) 0.046(16) Uiso 1 1 d . . . . .
H9 H -0.147(10) 0.091(10) 0.426(4) 0.028(13) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 O1 2.150(2) . ?
Mn1 O1 2.150(2) 2_566 ?
Mn1 O3 2.173(3) . ?
Mn1 O3 2.173(3) 2_566 ?
Mn1 O2 2.202(2) 2_666 ?
Mn1 O2 2.202(2) 1_455 ?
O2 C1 1.258(4) . ?
O2 Mn1 2.202(2) 1_655 ?
O1 C1 1.255(4) . ?
O3 H8 0.81(6) . ?
O3 H9 0.75(5) . ?
N1 C2 1.473(5) . ?
N1 C3 1.487(5) . ?
N1 H3 0.92(4) . ?
N1 H4 0.96(4) . ?
C1 C2 1.513(5) . ?
C2 H1 0.92(5) . ?
C2 H2 1.01(5) . ?
C3 H5 1.00(6) . ?
C3 H6 0.92(4) . ?
C3 H7 0.96(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Mn1 O1 180.0 . 2_566 ?
O1 Mn1 O3 85.20(11) . . ?
O1 Mn1 O3 94.80(11) 2_566 . ?
O1 Mn1 O3 94.80(11) . 2_566 ?
O1 Mn1 O3 85.20(11) 2_566 2_566 ?
O3 Mn1 O3 180.00(16) . 2_566 ?
O1 Mn1 O2 90.97(9) . 2_666 ?
O1 Mn1 O2 89.03(9) 2_566 2_666 ?
O3 Mn1 O2 89.43(10) . 2_666 ?
O3 Mn1 O2 90.57(10) 2_566 2_666 ?
O1 Mn1 O2 89.03(9) . 1_455 ?
O1 Mn1 O2 90.97(9) 2_566 1_455 ?
O3 Mn1 O2 90.57(10) . 1_455 ?
O3 Mn1 O2 89.43(10) 2_566 1_455 ?
O2 Mn1 O2 180.00(12) 2_666 1_455 ?
C1 O2 Mn1 127.2(2) . 1_655 ?
C1 O1 Mn1 128.9(2) . . ?
Mn1 O3 H8 122(4) . . ?
Mn1 O3 H9 124(4) . . ?
H8 O3 H9 111(5) . . ?
C2 N1 C3 113.2(3) . . ?
C2 N1 H3 109(2) . . ?
C3 N1 H3 111(2) . . ?
C2 N1 H4 108(2) . . ?
C3 N1 H4 105(2) . . ?
H3 N1 H4 110(3) . . ?
O1 C1 O2 125.7(3) . . ?
O1 C1 C2 117.1(3) . . ?
O2 C1 C2 117.2(3) . . ?
N1 C2 C1 112.4(3) . . ?
N1 C2 H1 109(3) . . ?
C1 C2 H1 108(3) . . ?
N1 C2 H2 106(3) . . ?
C1 C2 H2 106(3) . . ?
H1 C2 H2 114(4) . . ?
N1 C3 H5 110(3) . . ?
N1 C3 H6 103(2) . . ?
H5 C3 H6 118(4) . . ?
N1 C3 H7 109(3) . . ?
H5 C3 H7 105(4) . . ?
H6 C3 H7 113(4) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H3 Cl1 0.92(4) 2.26(4) 3.146(3) 162(3) .
N1 H4 Cl1 0.96(4) 2.15(4) 3.098(3) 167(3) 1_565

_refine_diff_density_max         0.556
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.098

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC12
_database_code_depnum_ccdc_archive 'CCDC 1841218'
_audit_update_record             
;
2018-05-03 deposited with the CCDC.
2018-06-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C9 H21 N3 O6 Sr, 2(Cl)'
_chemical_formula_sum            'C9 H21 Cl2 N3 O6 Sr'
_chemical_formula_weight         425.81

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Sr Sr -1.5307 3.2498 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      Monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/a'
_space_group_name_Hall           '-P 2yab'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x-1/2, -y-1/2, z'

_cell_length_a                   8.7535(6)
_cell_length_b                   10.3752(7)
_cell_length_c                   17.8337(13)
_cell_angle_alpha                90
_cell_angle_beta                 91.867(6)
_cell_angle_gamma                90
_cell_volume                     1618.8(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    906
_cell_measurement_theta_min      2.0
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_F_000             864
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    3.688
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.860
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
'The program SADABS-2008/1 - G.M. Sheldrick was used to apply a multi-scan absorption correction.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Tube'
_diffrn_measurement_device_type  'Rigaku Mercury2 (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 13.6612
_diffrn_reflns_number            16382
_diffrn_reflns_av_unetI/netI     0.0642
_diffrn_reflns_av_R_equivalents  0.0856
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.271
_diffrn_reflns_theta_max         27.506
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3726
_reflns_number_gt                2620
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3726
_refine_ls_number_parameters     274
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0390
_refine_ls_wR_factor_ref         0.1262
_refine_ls_wR_factor_gt          0.1001
_refine_ls_goodness_of_fit_ref   0.823
_refine_ls_restrained_S_all      0.823
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sr1 Sr 0.03099(4) 0.23953(3) 0.24534(2) 0.01241(14) Uani 1 1 d . . . . .
Cl1A Cl 0.49250(13) -0.28542(11) 0.41320(6) 0.0236(3) Uani 1 1 d . . . . .
Cl1B Cl 0.49550(13) -0.22258(11) 0.08388(6) 0.0228(3) Uani 1 1 d . . . . .
O1 O -0.0517(4) 0.0028(3) 0.2247(2) 0.0272(8) Uani 1 1 d . . . . .
O2 O -0.2700(5) 0.0887(4) 0.2603(2) 0.0367(10) Uani 1 1 d . . . . .
C1 C -0.1870(6) -0.0049(4) 0.2451(2) 0.0192(10) Uani 1 1 d . . . . .
C2 C -0.2595(6) -0.1368(5) 0.2496(3) 0.0194(10) Uani 1 1 d . . . . .
N1 N -0.1421(4) -0.2399(3) 0.2471(2) 0.0174(8) Uani 1 1 d . . . . .
C3 C -0.2103(7) -0.3699(5) 0.2506(3) 0.0305(12) Uani 1 1 d . . . . .
O3A O 0.1419(4) 0.1311(3) 0.36459(18) 0.0259(8) Uani 1 1 d . . . . .
O4A O 0.3897(4) 0.1478(4) 0.3405(2) 0.0360(9) Uani 1 1 d . . . . .
C4A C 0.2806(6) 0.1149(4) 0.3788(2) 0.0194(10) Uani 1 1 d . . . . .
C5A C 0.3276(5) 0.0455(4) 0.4508(2) 0.0165(9) Uani 1 1 d . . . . .
N2A N 0.1942(5) 0.0022(4) 0.4937(2) 0.0166(8) Uani 1 1 d . . . . .
C6A C 0.2384(7) -0.0759(6) 0.5596(3) 0.0328(13) Uani 1 1 d . . . . .
O3B O 0.2682(4) 0.1744(3) 0.17667(17) 0.0223(7) Uani 1 1 d . . . . .
O4B O 0.4702(4) 0.1329(4) 0.10954(19) 0.0273(8) Uani 1 1 d . . . . .
C4B C 0.3316(5) 0.1290(4) 0.1204(2) 0.0165(9) Uani 1 1 d . . . . .
C5B C 0.2216(5) 0.0677(5) 0.0619(3) 0.0184(9) Uani 1 1 d . . . . .
N2B N 0.3052(5) 0.0053(4) 0.0007(2) 0.0165(8) Uani 1 1 d . . . . .
C6B C 0.1988(6) -0.0551(5) -0.0558(3) 0.0232(11) Uani 1 1 d . . . . .
H1A H -0.316(7) -0.146(5) 0.294(3) 0.034(15) Uiso 1 1 d . . . . .
H1B H -0.328(7) -0.149(6) 0.206(4) 0.045(18) Uiso 1 1 d . . . . .
H2A H -0.071(5) -0.222(4) 0.289(3) 0.008(11) Uiso 1 1 d . . . . .
H2B H -0.094(6) -0.229(5) 0.206(3) 0.023(14) Uiso 1 1 d . . . . .
H3A H -0.284(7) -0.365(6) 0.293(4) 0.048(18) Uiso 1 1 d . . . . .
H3B H -0.283(7) -0.374(6) 0.210(4) 0.041(17) Uiso 1 1 d . . . . .
H4 H -0.129(8) -0.429(6) 0.241(4) 0.049(19) Uiso 1 1 d . . . . .
H5A H 0.382(5) -0.040(4) 0.437(2) 0.011(11) Uiso 1 1 d . . . . .
H6A H 0.391(5) 0.102(4) 0.486(3) 0.013(12) Uiso 1 1 d . . . . .
H7A H 0.128(6) -0.050(5) 0.462(3) 0.018(13) Uiso 1 1 d . . . . .
H8A H 0.140(7) 0.064(6) 0.508(3) 0.035(17) Uiso 1 1 d . . . . .
H9A H 0.296(6) -0.150(5) 0.541(3) 0.019(13) Uiso 1 1 d . . . . .
H10A H 0.299(7) -0.039(6) 0.588(3) 0.028(17) Uiso 1 1 d . . . . .
H11A H 0.140(7) -0.091(6) 0.588(4) 0.051(19) Uiso 1 1 d . . . . .
H5B H 0.159(6) -0.009(5) 0.084(3) 0.034(15) Uiso 1 1 d . . . . .
H6B H 0.154(6) 0.139(5) 0.041(3) 0.028(14) Uiso 1 1 d . . . . .
H7B H 0.368(6) -0.052(6) 0.015(3) 0.030(16) Uiso 1 1 d . . . . .
H8B H 0.370(8) 0.069(7) -0.019(4) 0.06(2) Uiso 1 1 d . . . . .
H9B H 0.137(7) -0.120(6) -0.030(3) 0.037(16) Uiso 1 1 d . . . . .
H10B H 0.137(7) 0.008(6) -0.075(3) 0.040(17) Uiso 1 1 d . . . . .
H11B H 0.248(6) -0.082(5) -0.090(3) 0.025(15) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sr1 O4A 2.431(3) 4_565 ?
Sr1 O2 2.500(3) 4_665 ?
Sr1 O3B 2.537(3) . ?
Sr1 O3A 2.568(3) . ?
Sr1 O1 2.583(3) . ?
Sr1 O3B 2.721(3) 4_565 ?
Sr1 O4B 2.796(3) 4_565 ?
Sr1 O2 3.084(4) . ?
Sr1 C4B 3.101(4) 4_565 ?
Sr1 C1 3.174(5) . ?
Sr1 Sr1 4.3821(3) 4_665 ?
Sr1 Sr1 4.3821(3) 4_565 ?
O1 C1 1.254(6) . ?
O2 C1 1.248(6) . ?
O2 Sr1 2.500(3) 4_565 ?
C1 C2 1.511(6) . ?
C2 N1 1.485(6) . ?
N1 C3 1.478(6) . ?
O3A C4A 1.244(6) . ?
O4A C4A 1.240(6) . ?
O4A Sr1 2.431(3) 4_665 ?
C4A C5A 1.516(6) . ?
C5A N2A 1.487(6) . ?
N2A C6A 1.468(6) . ?
O3B C4B 1.254(5) . ?
O3B Sr1 2.721(3) 4_665 ?
O4B C4B 1.235(5) . ?
O4B Sr1 2.796(3) 4_665 ?
C4B C5B 1.535(6) . ?
C4B Sr1 3.101(4) 4_665 ?
C5B N2B 1.483(6) . ?
N2B C6B 1.488(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4A Sr1 O2 87.19(14) 4_565 4_665 ?
O4A Sr1 O3B 155.23(12) 4_565 . ?
O2 Sr1 O3B 70.32(12) 4_665 . ?
O4A Sr1 O3A 79.62(12) 4_565 . ?
O2 Sr1 O3A 88.88(12) 4_665 . ?
O3B Sr1 O3A 89.41(11) . . ?
O4A Sr1 O1 114.22(13) 4_565 . ?
O2 Sr1 O1 152.11(13) 4_665 . ?
O3B Sr1 O1 84.71(11) . . ?
O3A Sr1 O1 78.37(11) . . ?
O4A Sr1 O3B 73.42(11) 4_565 4_565 ?
O2 Sr1 O3B 112.95(12) 4_665 4_565 ?
O3B Sr1 O3B 124.30(12) . 4_565 ?
O3A Sr1 O3B 143.86(10) . 4_565 ?
O1 Sr1 O3B 91.09(10) . 4_565 ?
O4A Sr1 O4B 106.87(12) 4_565 4_565 ?
O2 Sr1 O4B 82.39(11) 4_665 4_565 ?
O3B Sr1 O4B 81.01(10) . 4_565 ?
O3A Sr1 O4B 168.76(11) . 4_565 ?
O1 Sr1 O4B 106.37(11) . 4_565 ?
O3B Sr1 O4B 47.19(9) 4_565 4_565 ?
O4A Sr1 O2 74.21(12) 4_565 . ?
O2 Sr1 O2 161.20(12) 4_665 . ?
O3B Sr1 O2 128.47(10) . . ?
O3A Sr1 O2 90.40(10) . . ?
O1 Sr1 O2 45.07(10) . . ?
O3B Sr1 O2 59.57(9) 4_565 . ?
O4B Sr1 O2 100.15(10) 4_565 . ?
O4A Sr1 C4B 90.16(12) 4_565 4_565 ?
O2 Sr1 C4B 97.89(12) 4_665 4_565 ?
O3B Sr1 C4B 102.76(11) . 4_565 ?
O3A Sr1 C4B 167.48(11) . 4_565 ?
O1 Sr1 C4B 99.62(11) . 4_565 ?
O3B Sr1 C4B 23.73(10) 4_565 4_565 ?
O4B Sr1 C4B 23.46(10) 4_565 4_565 ?
O2 Sr1 C4B 79.80(10) . 4_565 ?
O4A Sr1 C1 93.76(13) 4_565 . ?
O2 Sr1 C1 170.57(12) 4_665 . ?
O3B Sr1 C1 106.75(11) . . ?
O3A Sr1 C1 82.07(11) . . ?
O1 Sr1 C1 22.27(11) . . ?
O3B Sr1 C1 76.25(11) 4_565 . ?
O4B Sr1 C1 106.24(11) 4_565 . ?
O2 Sr1 C1 22.95(10) . . ?
C4B Sr1 C1 91.50(11) 4_565 . ?
O4A Sr1 Sr1 120.45(10) 4_565 4_665 ?
O2 Sr1 Sr1 43.32(10) 4_665 4_665 ?
O3B Sr1 Sr1 34.90(7) . 4_665 ?
O3A Sr1 Sr1 70.80(8) . 4_665 ?
O1 Sr1 Sr1 108.80(8) . 4_665 ?
O3B Sr1 Sr1 144.42(7) 4_565 4_665 ?
O4B Sr1 Sr1 97.97(7) 4_565 4_665 ?
O2 Sr1 Sr1 151.81(6) . 4_665 ?
C4B Sr1 Sr1 121.13(8) 4_565 4_665 ?
C1 Sr1 Sr1 129.80(8) . 4_665 ?
O4A Sr1 Sr1 56.32(9) 4_565 4_565 ?
O2 Sr1 Sr1 131.06(10) 4_665 4_565 ?
O3B Sr1 Sr1 147.85(7) . 4_565 ?
O3A Sr1 Sr1 111.86(8) . 4_565 ?
O1 Sr1 Sr1 76.82(8) . 4_565 ?
O3B Sr1 Sr1 32.23(6) 4_565 4_565 ?
O4B Sr1 Sr1 79.31(7) 4_565 4_565 ?
O2 Sr1 Sr1 33.79(6) . 4_565 ?
C4B Sr1 Sr1 55.90(8) 4_565 4_565 ?
C1 Sr1 Sr1 55.89(8) . 4_565 ?
Sr1 Sr1 Sr1 174.314(18) 4_665 4_565 ?
C1 O1 Sr1 106.4(3) . . ?
C1 O2 Sr1 160.0(3) . 4_565 ?
C1 O2 Sr1 82.6(3) . . ?
Sr1 O2 Sr1 102.89(13) 4_565 . ?
O2 C1 O1 125.2(4) . . ?
O2 C1 C2 116.4(4) . . ?
O1 C1 C2 118.4(4) . . ?
O2 C1 Sr1 74.5(3) . . ?
O1 C1 Sr1 51.3(2) . . ?
C2 C1 Sr1 167.6(3) . . ?
N1 C2 C1 111.0(4) . . ?
C3 N1 C2 112.1(4) . . ?
C4A O3A Sr1 124.6(3) . . ?
C4A O4A Sr1 159.3(4) . 4_665 ?
O4A C4A O3A 127.9(4) . . ?
O4A C4A C5A 113.9(4) . . ?
O3A C4A C5A 118.2(4) . . ?
N2A C5A C4A 112.5(4) . . ?
C6A N2A C5A 112.8(4) . . ?
C4B O3B Sr1 151.2(3) . . ?
C4B O3B Sr1 95.4(3) . 4_665 ?
Sr1 O3B Sr1 112.87(11) . 4_665 ?
C4B O4B Sr1 92.3(3) . 4_665 ?
O4B C4B O3B 125.1(4) . . ?
O4B C4B C5B 120.3(4) . . ?
O3B C4B C5B 114.6(4) . . ?
O4B C4B Sr1 64.3(2) . 4_665 ?
O3B C4B Sr1 60.9(2) . 4_665 ?
C5B C4B Sr1 175.4(3) . 4_665 ?
N2B C5B C4B 111.6(4) . . ?
C5B N2B C6B 111.6(4) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H2A Cl1A 0.98(5) 2.27(5) 3.163(4) 153(4) 4
N1 H2B Cl1B 0.86(6) 2.39(6) 3.210(4) 158(5) 4
N2A H7A Cl1A 0.97(5) 2.24(5) 3.173(4) 163(4) 4
N2A H8A Cl1A 0.84(6) 2.42(6) 3.234(4) 163(5) 2_556
N2B H7B Cl1B 0.84(6) 2.41(6) 3.226(4) 164(5) .
N2B H8B Cl1B 0.94(7) 2.31(7) 3.251(4) 172(6) 3_655

_refine_diff_density_max         0.840
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.114

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC13
_database_code_depnum_ccdc_archive 'CCDC 1841217'
_audit_update_record             
;
2018-05-03 deposited with the CCDC.
2018-06-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C9 H21 N3 O6 Sr, 2(Br)'
_chemical_formula_sum            'C9 H21 Br2 N3 O6 Sr'
_chemical_formula_weight         514.73

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Sr Sr -1.5307 3.2498 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      Orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P cab'
_space_group_name_Hall           '-P 2bc 2ac'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y+1/2, z+1/2'
'x+1/2, -y, -z+1/2'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'-x-1/2, y, z-1/2'
'x-1/2, -y-1/2, z'

_cell_length_a                   8.8611(6)
_cell_length_b                   10.5404(7)
_cell_length_c                   36.6110(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3419.5(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    893
_cell_measurement_theta_min      1.7
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.000
_exptl_crystal_F_000             2016
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    7.854
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.771
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
'The program SADABS-2008/1 - G.M. Sheldrick was used to apply a multi-scan absorption correction.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Tube'
_diffrn_measurement_device_type  'Rigaku Mercury2 (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 13.6612
_diffrn_reflns_number            31978
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_av_R_equivalents  0.0815
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_theta_min         2.225
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3923
_reflns_number_gt                2664
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3923
_refine_ls_number_parameters     274
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0845
_refine_ls_R_factor_gt           0.0501
_refine_ls_wR_factor_ref         0.1782
_refine_ls_wR_factor_gt          0.1551
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_restrained_S_all      1.165
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sr2 Sr 0.04518(7) -0.26009(5) 0.62479(2) 0.0206(2) Uani 1 1 d . . . . .
Br1A Br 0.00657(7) 0.27823(8) 0.54351(2) 0.0368(2) Uani 1 1 d . . . . .
Br1B Br 0.03484(9) 0.24684(6) 0.70909(2) 0.0340(2) Uani 1 1 d . . . . .
O1 O 0.2382(8) -0.0900(5) 0.61745(15) 0.076(2) Uani 1 1 d . . . . .
O2 O 0.4557(7) -0.0088(5) 0.63483(15) 0.0509(13) Uani 1 1 d . . . . .
C1 C 0.3242(10) -0.0008(6) 0.62558(16) 0.0382(18) Uani 1 1 d . . . . .
C2 C 0.2521(7) 0.1310(6) 0.62452(19) 0.0313(14) Uani 1 1 d . . . . .
N1 N 0.3679(6) 0.2315(5) 0.62701(15) 0.0281(11) Uani 1 1 d . . . . .
C3 C 0.3050(11) 0.3610(7) 0.6263(2) 0.0432(19) Uani 1 1 d . . . . .
O3A O -0.1175(7) -0.1471(6) 0.58206(16) 0.0739(19) Uani 1 1 d . . . . .
O4A O -0.3581(6) -0.1384(5) 0.56539(13) 0.0520(14) Uani 1 1 d . . . . .
C4A C -0.2208(9) -0.1182(6) 0.56101(19) 0.0356(16) Uani 1 1 d . . . . .
C5A C -0.1701(7) -0.0487(7) 0.52696(17) 0.0290(14) Uani 1 1 d . . . . .
N2A N -0.2995(6) -0.0087(5) 0.50421(14) 0.0278(11) Uani 1 1 d . . . . .
C6A C -0.2563(11) 0.0638(9) 0.4713(2) 0.043(2) Uani 1 1 d . . . . .
O3B O 0.2702(6) -0.3266(5) 0.66201(14) 0.0560(15) Uani 1 1 d . . . . .
O4B O 0.4893(6) -0.3631(6) 0.68660(15) 0.0661(18) Uani 1 1 d . . . . .
C4B C 0.3516(8) -0.3704(6) 0.68656(18) 0.0329(15) Uani 1 1 d . . . . .
C5B C 0.2727(7) -0.4359(6) 0.71782(18) 0.0294(14) Uani 1 1 d . . . . .
N2B N 0.3818(7) -0.4863(5) 0.74473(15) 0.0308(12) Uani 1 1 d . . . . .
C6B C 0.3095(10) -0.5510(8) 0.7764(2) 0.0436(19) Uani 1 1 d . . . . .
H1A H 0.201(7) 0.138(7) 0.600(2) 0.041(19) Uiso 1 1 d . . . . .
H1B H 0.172(9) 0.155(8) 0.642(2) 0.06(3) Uiso 1 1 d . . . . .
H2A H 0.440(7) 0.217(6) 0.6040(18) 0.031(17) Uiso 1 1 d . . . . .
H2B H 0.431(10) 0.218(9) 0.645(3) 0.08(3) Uiso 1 1 d . . . . .
H3A H 0.247(8) 0.357(6) 0.6071(19) 0.031(19) Uiso 1 1 d . . . . .
H3B H 0.237(9) 0.380(7) 0.645(2) 0.05(2) Uiso 1 1 d . . . . .
H4 H 0.367(16) 0.425(15) 0.622(3) 0.15(6) Uiso 1 1 d . . . . .
H5A H -0.100(7) 0.028(7) 0.5340(17) 0.036(18) Uiso 1 1 d . . . . .
H6A H -0.112(7) -0.101(6) 0.5153(18) 0.030(18) Uiso 1 1 d . . . . .
H7A H -0.385(7) 0.043(6) 0.5207(17) 0.038(18) Uiso 1 1 d . . . . .
H8A H -0.350(7) -0.073(6) 0.4970(17) 0.028(18) Uiso 1 1 d . . . . .
H9A H -0.211(7) 0.138(7) 0.4777(18) 0.028(18) Uiso 1 1 d . . . . .
H10A H -0.212(7) 0.021(6) 0.4540(18) 0.026(18) Uiso 1 1 d . . . . .
H11A H -0.322(8) 0.084(7) 0.456(2) 0.04(2) Uiso 1 1 d . . . . .
H5B H 0.203(8) -0.383(7) 0.733(2) 0.05(2) Uiso 1 1 d . . . . .
H6B H 0.195(8) -0.514(7) 0.7127(18) 0.04(2) Uiso 1 1 d . . . . .
H7B H 0.442(6) -0.428(6) 0.7504(15) 0.013(14) Uiso 1 1 d . . . . .
H8B H 0.435(7) -0.547(6) 0.7325(16) 0.024(16) Uiso 1 1 d . . . . .
H9B H 0.246(9) -0.502(8) 0.790(2) 0.05(2) Uiso 1 1 d . . . . .
H10B H 0.250(8) -0.639(7) 0.7709(18) 0.04(2) Uiso 1 1 d . . . . .
H11B H 0.371(12) -0.573(11) 0.792(3) 0.10(4) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sr2 O3A 2.438(5) . ?
Sr2 O1 2.492(6) . ?
Sr2 O3B 2.515(5) . ?
Sr2 O4A 2.570(5) 8_655 ?
Sr2 O2 2.587(5) 8 ?
Sr2 O4B 2.656(5) 8 ?
Sr2 O3B 2.937(6) 8 ?
Sr2 C4B 3.154(7) 8 ?
Sr2 O1 3.157(8) 8 ?
Sr2 C1 3.192(8) 8 ?
Sr2 C4A 3.376(7) 8_655 ?
Sr2 Sr2 4.4356(3) 8_655 ?
O1 C1 1.247(9) . ?
O1 Sr2 3.157(8) 8_655 ?
O2 C1 1.216(9) . ?
O2 Sr2 2.588(5) 8_655 ?
C1 C2 1.529(10) . ?
C1 Sr2 3.192(8) 8_655 ?
C2 N1 1.477(8) . ?
N1 C3 1.476(8) . ?
O3A C4A 1.235(9) . ?
O4A C4A 1.246(9) . ?
O4A Sr2 2.570(5) 8 ?
C4A C5A 1.514(9) . ?
C4A Sr2 3.376(7) 8 ?
C5A N2A 1.479(8) . ?
N2A C6A 1.476(8) . ?
O3B C4B 1.241(8) . ?
O3B Sr2 2.937(6) 8_655 ?
O4B C4B 1.223(8) . ?
O4B Sr2 2.656(5) 8_655 ?
C4B C5B 1.508(9) . ?
C4B Sr2 3.154(7) 8_655 ?
C5B N2B 1.479(8) . ?
N2B C6B 1.489(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3A Sr2 O1 89.1(2) . . ?
O3A Sr2 O3B 162.3(2) . . ?
O1 Sr2 O3B 73.4(2) . . ?
O3A Sr2 O4A 81.8(2) . 8_655 ?
O1 Sr2 O4A 88.81(18) . 8_655 ?
O3B Sr2 O4A 94.48(19) . 8_655 ?
O3A Sr2 O2 111.7(2) . 8 ?
O1 Sr2 O2 154.5(2) . 8 ?
O3B Sr2 O2 84.46(19) . 8 ?
O4A Sr2 O2 80.25(17) 8_655 8 ?
O3A Sr2 O4B 101.4(2) . 8 ?
O1 Sr2 O4B 82.43(19) . 8 ?
O3B Sr2 O4B 79.77(18) . 8 ?
O4A Sr2 O4B 170.59(17) 8_655 8 ?
O2 Sr2 O4B 106.4(2) 8 8 ?
O3A Sr2 O3B 69.84(19) . 8 ?
O1 Sr2 O3B 113.3(2) . 8 ?
O3B Sr2 O3B 119.5(2) . 8 ?
O4A Sr2 O3B 142.98(16) 8_655 8 ?
O2 Sr2 O3B 88.45(17) 8 8 ?
O4B Sr2 O3B 45.40(14) 8 8 ?
O3A Sr2 C4B 85.7(2) . 8 ?
O1 Sr2 C4B 97.87(19) . 8 ?
O3B Sr2 C4B 99.46(18) . 8 ?
O4A Sr2 C4B 165.77(17) 8_655 8 ?
O2 Sr2 C4B 98.16(17) 8 8 ?
O4B Sr2 C4B 22.25(15) 8 8 ?
O3B Sr2 C4B 23.16(15) 8 8 ?
O3A Sr2 O1 71.37(19) . 8 ?
O1 Sr2 O1 160.4(2) . 8 ?
O3B Sr2 O1 126.13(17) . 8 ?
O4A Sr2 O1 90.40(16) 8_655 8 ?
O2 Sr2 O1 43.71(16) 8 8 ?
O4B Sr2 O1 99.00(16) 8 8 ?
O3B Sr2 O1 58.70(14) 8 8 ?
C4B Sr2 O1 79.08(15) 8 8 ?
O3A Sr2 C1 91.7(2) . 8 ?
O1 Sr2 C1 171.89(19) . 8 ?
O3B Sr2 C1 105.14(18) . 8 ?
O4A Sr2 C1 83.32(16) 8_655 8 ?
O2 Sr2 C1 21.17(16) 8 8 ?
O4B Sr2 C1 105.30(18) 8 8 ?
O3B Sr2 C1 74.49(16) 8 8 ?
C4B Sr2 C1 90.23(16) 8 8 ?
O1 Sr2 C1 22.64(16) 8 8 ?
O3A Sr2 C4A 96.0(2) . 8_655 ?
O1 Sr2 C4A 77.13(19) . 8_655 ?
O3B Sr2 C4A 77.40(18) . 8_655 ?
O4A Sr2 C4A 18.56(17) 8_655 8_655 ?
O2 Sr2 C4A 85.90(16) 8 8_655 ?
O4B Sr2 C4A 152.84(17) 8 8_655 ?
O3B Sr2 C4A 161.54(16) 8 8_655 ?
C4B Sr2 C4A 174.65(17) 8 8_655 ?
O1 Sr2 C4A 106.27(15) 8 8_655 ?
C1 Sr2 C4A 94.76(16) 8 8_655 ?
O3A Sr2 Sr2 124.55(16) . 8_655 ?
O1 Sr2 Sr2 43.94(18) . 8_655 ?
O3B Sr2 Sr2 38.87(13) . 8_655 ?
O4A Sr2 Sr2 71.76(13) 8_655 8_655 ?
O2 Sr2 Sr2 110.55(13) 8 8_655 ?
O4B Sr2 Sr2 99.37(11) 8 8_655 ?
O3B Sr2 Sr2 144.44(9) 8 8_655 ?
C4B Sr2 Sr2 121.49(12) 8 8_655 ?
O1 Sr2 Sr2 152.20(9) 8 8_655 ?
C1 Sr2 Sr2 130.59(13) 8 8_655 ?
C4A Sr2 Sr2 53.47(12) 8_655 8_655 ?
C1 O1 Sr2 159.5(5) . . ?
C1 O1 Sr2 80.2(5) . 8_655 ?
Sr2 O1 Sr2 102.8(2) . 8_655 ?
C1 O2 Sr2 108.6(5) . 8_655 ?
O2 C1 O1 126.8(8) . . ?
O2 C1 C2 118.1(6) . . ?
O1 C1 C2 115.1(7) . . ?
O2 C1 Sr2 50.2(4) . 8_655 ?
O1 C1 Sr2 77.1(5) . 8_655 ?
C2 C1 Sr2 166.7(5) . 8_655 ?
N1 C2 C1 111.1(5) . . ?
C3 N1 C2 113.6(6) . . ?
C4A O3A Sr2 163.6(6) . . ?
C4A O4A Sr2 120.4(4) . 8 ?
O3A C4A O4A 127.0(7) . . ?
O3A C4A C5A 114.4(7) . . ?
O4A C4A C5A 118.6(6) . . ?
O3A C4A Sr2 86.0(5) . 8 ?
O4A C4A Sr2 41.0(3) . 8 ?
C5A C4A Sr2 159.3(5) . 8 ?
N2A C5A C4A 111.8(5) . . ?
C6A N2A C5A 114.0(6) . . ?
C4B O3B Sr2 163.0(5) . . ?
C4B O3B Sr2 88.3(4) . 8_655 ?
Sr2 O3B Sr2 108.63(17) . 8_655 ?
C4B O4B Sr2 102.5(4) . 8_655 ?
O4B C4B O3B 123.8(7) . . ?
O4B C4B C5B 119.4(6) . . ?
O3B C4B C5B 116.8(6) . . ?
O4B C4B Sr2 55.3(3) . 8_655 ?
O3B C4B Sr2 68.6(4) . 8_655 ?
C5B C4B Sr2 174.6(5) . 8_655 ?
N2B C5B C4B 111.5(5) . . ?
C5B N2B C6B 113.7(6) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H2A Br1A 1.07(6) 2.29(7) 3.296(5) 156(5) 8_665
N1 H2B Br1B 0.87(9) 2.55(10) 3.357(6) 154(8) 8_665
N2A H7A Br1A 1.11(7) 2.28(7) 3.305(6) 153(5) 8_565
N2A H8A Br1A 0.85(6) 2.57(7) 3.386(6) 161(6) 4_446
N2B H7B Br1B 0.84(6) 2.55(6) 3.327(6) 153(5) 3_556
N2B H8B Br1B 0.91(6) 2.44(6) 3.329(6) 165(5) 8_655

_refine_diff_density_max         1.574
_refine_diff_density_min         -1.696
_refine_diff_density_rms         0.154

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC14
_database_code_depnum_ccdc_archive 'CCDC 1841204'
_audit_update_record             
;
2018-05-03 deposited with the CCDC.
2018-06-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H18 Mg N2 O6, 2(Cl)'
_chemical_formula_sum            'C6 H18 Cl2 Mg N2 O6'
_chemical_formula_weight         309.43

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   4.7825(5)
_cell_length_b                   5.3422(5)
_cell_length_c                   13.6722(14)
_cell_angle_alpha                84.343(17)
_cell_angle_beta                 80.426(17)
_cell_angle_gamma                88.026(17)
_cell_volume                     342.71(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    826
_cell_measurement_theta_min      1.5
_cell_measurement_theta_max      27.5

_exptl_crystal_description       platelet
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_F_000             162
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    0.536
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.521
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
'The program SADABS-2008/1 - G.M. Sheldrick was used to apply a multi-scan absorption correction.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Tube'
_diffrn_measurement_device_type  'Rigaku Mercury2 (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 13.6612
_diffrn_reflns_number            3529
_diffrn_reflns_av_unetI/netI     0.0792
_diffrn_reflns_av_R_equivalents  0.0600
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.036
_diffrn_reflns_theta_max         27.495
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             1560
_reflns_number_gt                998
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1560
_refine_ls_number_parameters     96
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.1018
_refine_ls_R_factor_gt           0.0648
_refine_ls_wR_factor_ref         0.2299
_refine_ls_wR_factor_gt          0.2188
_refine_ls_goodness_of_fit_ref   1.335
_refine_ls_restrained_S_all      1.334
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mg1 Mg 0.0000 0.5000 0.5000 0.0257(6) Uani 1 2 d S . P . .
Cl1 Cl 0.2241(3) 0.2238(2) 0.17971(11) 0.0421(5) Uani 1 1 d . . . . .
O2 O 0.6785(7) 0.7234(6) 0.4452(3) 0.0317(8) Uani 1 1 d . . . . .
O1 O 0.2914(7) 0.6484(6) 0.3811(3) 0.0308(8) Uani 1 1 d . . . . .
O3 O -0.0617(8) 0.2178(6) 0.4122(3) 0.0357(9) Uani 1 1 d D . . . .
N1 N 0.5526(9) 0.7143(8) 0.1907(3) 0.0320(10) Uani 1 1 d D . . . .
C1 C 0.5486(10) 0.6971(8) 0.3738(4) 0.0267(10) Uani 1 1 d . . . . .
C2 C 0.7210(10) 0.7240(10) 0.2719(4) 0.0334(12) Uani 1 1 d . . . . .
H2A H 0.8183 0.8830 0.2626 0.040 Uiso 1 1 calc R U . . .
H2B H 0.8641 0.5906 0.2672 0.040 Uiso 1 1 calc R U . . .
C3 C 0.7227(14) 0.7322(13) 0.0902(4) 0.0513(16) Uani 1 1 d . . . . .
H3A H 0.8236 0.8874 0.0785 0.077 Uiso 1 1 calc R U . . .
H3B H 0.5998 0.7274 0.0416 0.077 Uiso 1 1 calc R U . . .
H3C H 0.8556 0.5935 0.0850 0.077 Uiso 1 1 calc R U . . .
H3 H 0.434(9) 0.565(7) 0.208(4) 0.031(14) Uiso 1 1 d D . . . .
H4 H 0.408(10) 0.846(9) 0.204(5) 0.06(2) Uiso 1 1 d D . . . .
H8 H 0.062(10) 0.183(11) 0.351(3) 0.052(18) Uiso 1 1 d D . . . .
H9 H -0.215(11) 0.101(12) 0.438(6) 0.09(3) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mg1 O1 2.069(3) . ?
Mg1 O1 2.069(3) 2_566 ?
Mg1 O3 2.075(3) 2_566 ?
Mg1 O3 2.075(3) . ?
Mg1 O2 2.105(4) 1_455 ?
Mg1 O2 2.105(4) 2_666 ?
O2 C1 1.262(6) . ?
O2 Mg1 2.105(4) 1_655 ?
O1 C1 1.252(5) . ?
O3 H8 0.97(2) . ?
O3 H9 0.98(2) . ?
N1 C3 1.472(7) . ?
N1 C2 1.482(7) . ?
N1 H3 0.983(19) . ?
N1 H4 0.98(2) . ?
C1 C2 1.492(7) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Mg1 O1 180.0 . 2_566 ?
O1 Mg1 O3 92.84(14) . 2_566 ?
O1 Mg1 O3 87.16(14) 2_566 2_566 ?
O1 Mg1 O3 87.16(14) . . ?
O1 Mg1 O3 92.85(14) 2_566 . ?
O3 Mg1 O3 180.0 2_566 . ?
O1 Mg1 O2 89.62(13) . 1_455 ?
O1 Mg1 O2 90.38(13) 2_566 1_455 ?
O3 Mg1 O2 89.14(14) 2_566 1_455 ?
O3 Mg1 O2 90.85(14) . 1_455 ?
O1 Mg1 O2 90.38(13) . 2_666 ?
O1 Mg1 O2 89.62(13) 2_566 2_666 ?
O3 Mg1 O2 90.86(14) 2_566 2_666 ?
O3 Mg1 O2 89.15(14) . 2_666 ?
O2 Mg1 O2 180.00(18) 1_455 2_666 ?
C1 O2 Mg1 130.4(3) . 1_655 ?
C1 O1 Mg1 131.7(3) . . ?
Mg1 O3 H8 125(4) . . ?
Mg1 O3 H9 118(5) . . ?
H8 O3 H9 117(6) . . ?
C3 N1 C2 114.2(4) . . ?
C3 N1 H3 116(3) . . ?
C2 N1 H3 106(3) . . ?
C3 N1 H4 117(4) . . ?
C2 N1 H4 103(4) . . ?
H3 N1 H4 100(5) . . ?
O1 C1 O2 125.9(5) . . ?
O1 C1 C2 117.7(4) . . ?
O2 C1 C2 116.3(4) . . ?
N1 C2 C1 113.9(4) . . ?
N1 C2 H2A 108.8 . . ?
C1 C2 H2A 108.8 . . ?
N1 C2 H2B 108.8 . . ?
C1 C2 H2B 108.8 . . ?
H2A C2 H2B 107.7 . . ?
N1 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H3 Cl1 0.983(19) 2.21(3) 3.130(4) 156(4) .
N1 H4 Cl1 0.98(2) 2.19(3) 3.098(5) 154(5) 1_565

_refine_diff_density_max         0.515
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.099

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC15
_database_code_depnum_ccdc_archive 'CCDC 1841206'
_audit_update_record             
;
2018-05-03 deposited with the CCDC.
2018-06-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C9 H21 Ca N3 O6, 2(Br)'
_chemical_formula_sum            'C9 H21 Br2 Ca N3 O6'
_chemical_formula_weight         467.19

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   9.2414(6)
_cell_length_b                   17.6966(13)
_cell_length_c                   10.3565(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1693.7(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    922
_cell_measurement_theta_min      2.0
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.832
_exptl_crystal_F_000             936
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.77
_exptl_crystal_size_mid          0.69
_exptl_crystal_size_min          0.22
_exptl_absorpt_coefficient_mu    5.115
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.585
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
'The program SADABS-2008/1 - G.M. Sheldrick was used to apply a multi-scan absorption correction.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Tube'
_diffrn_measurement_device_type  'Rigaku Mercury2 (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 13.6612
_diffrn_reflns_number            15967
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.279
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measured_fraction_theta_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_point_group_measured_fraction_full 0.977
_reflns_number_total             1969
_reflns_number_gt                1683
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1969
_refine_ls_number_parameters     149
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0274
_refine_ls_wR_factor_ref         0.0957
_refine_ls_wR_factor_gt          0.0902
_refine_ls_goodness_of_fit_ref   0.799
_refine_ls_restrained_S_all      0.799
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.00793(3) 0.08313(2) 0.71984(2) 0.01962(14) Uani 1 1 d . . . . .
Ca1 Ca 0.46459(7) 0.2500 0.22097(5) 0.01034(16) Uani 1 2 d S T P . .
O3 O 0.83968(16) 0.35361(8) 0.37453(14) 0.0248(3) Uani 1 1 d . . . . .
O2 O 0.0999(2) 0.2500 0.47308(18) 0.0208(4) Uani 1 2 d S T P . .
O1 O 0.3314(2) 0.2500 0.4092(2) 0.0296(5) Uani 1 2 d S T P . .
O4 O 0.60796(18) 0.33961(9) 0.31704(16) 0.0315(4) Uani 1 1 d . . . . .
N1 N 0.1640(3) 0.2500 0.7232(2) 0.0157(5) Uani 1 2 d S T P . .
N2 N 0.7939(2) 0.48639(9) 0.49158(16) 0.0169(4) Uani 1 1 d . . . . .
C4 C 0.7105(2) 0.37220(10) 0.37138(16) 0.0161(4) Uani 1 1 d . . . . .
C1 C 0.2326(3) 0.2500 0.4913(2) 0.0158(5) Uani 1 2 d S T P . .
C5 C 0.6665(2) 0.44366(10) 0.44312(19) 0.0163(4) Uani 1 1 d . . . . .
C2 C 0.2855(3) 0.2500 0.6303(2) 0.0153(5) Uani 1 2 d S T P . .
C6 C 0.7540(3) 0.55506(12) 0.5662(2) 0.0287(5) Uani 1 1 d . . . . .
C3 C 0.2133(4) 0.2500 0.8610(3) 0.0250(6) Uani 1 2 d S T P . .
H1 H 0.346(3) 0.2926(13) 0.646(2) 0.021(6) Uiso 1 1 d . . . . .
H2 H 0.106(3) 0.2894(14) 0.710(2) 0.023(6) Uiso 1 1 d . . . . .
H3 H 0.268(3) 0.2914(16) 0.877(2) 0.027(7) Uiso 1 1 d . . . . .
H4 H 0.136(5) 0.2500 0.926(4) 0.047(12) Uiso 1 2 d S . P . .
H5 H 0.611(3) 0.4309(13) 0.520(3) 0.025(6) Uiso 1 1 d . . . . .
H6 H 0.618(3) 0.4744(14) 0.391(2) 0.021(6) Uiso 1 1 d . . . . .
H7 H 0.846(3) 0.4501(14) 0.542(3) 0.026(6) Uiso 1 1 d . . . . .
H8 H 0.843(3) 0.4993(17) 0.429(3) 0.037(7) Uiso 1 1 d . . . . .
H9 H 0.710(3) 0.5875(14) 0.508(3) 0.019(6) Uiso 1 1 d . . . . .
H10 H 0.703(3) 0.5410(15) 0.644(3) 0.031(7) Uiso 1 1 d . . . . .
H11 H 0.843(5) 0.5807(18) 0.591(4) 0.066(12) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ca1 O4 2.2935(15) . ?
Ca1 O4 2.2936(15) 7_565 ?
Ca1 O1 2.305(2) . ?
Ca1 O2 2.3671(19) 6_656 ?
Ca1 O3 2.3816(14) 4_455 ?
Ca1 O3 2.3816(14) 6_556 ?
O3 C4 1.239(2) . ?
O3 Ca1 2.3816(14) 6_656 ?
O2 C1 1.240(3) . ?
O2 Ca1 2.3671(19) 6_556 ?
O1 C1 1.248(3) . ?
O4 C4 1.244(2) . ?
N1 C2 1.479(4) . ?
N1 C3 1.498(4) . ?
N1 H2 0.89(3) . ?
N2 C6 1.487(2) . ?
N2 C5 1.487(3) . ?
N2 H7 0.96(3) . ?
N2 H8 0.82(3) . ?
C4 C5 1.522(3) . ?
C1 C2 1.521(3) . ?
C5 H5 0.97(3) . ?
C5 H6 0.88(2) . ?
C2 H1 0.95(2) . ?
C6 H9 0.93(3) . ?
C6 H10 0.96(3) . ?
C6 H11 0.98(4) . ?
C3 H3 0.91(3) . ?
C3 H4 0.98(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Ca1 O4 87.49(9) . 7_565 ?
O4 Ca1 O1 86.66(6) . . ?
O4 Ca1 O1 86.66(6) 7_565 . ?
O4 Ca1 O2 93.62(6) . 6_656 ?
O4 Ca1 O2 93.62(6) 7_565 6_656 ?
O1 Ca1 O2 179.62(8) . 6_656 ?
O4 Ca1 O3 172.94(6) . 4_455 ?
O4 Ca1 O3 85.86(6) 7_565 4_455 ?
O1 Ca1 O3 95.29(5) . 4_455 ?
O2 Ca1 O3 84.46(5) 6_656 4_455 ?
O4 Ca1 O3 85.86(6) . 6_556 ?
O4 Ca1 O3 172.94(6) 7_565 6_556 ?
O1 Ca1 O3 95.29(5) . 6_556 ?
O2 Ca1 O3 84.46(5) 6_656 6_556 ?
O3 Ca1 O3 100.68(8) 4_455 6_556 ?
C4 O3 Ca1 131.34(13) . 6_656 ?
C1 O2 Ca1 130.64(17) . 6_556 ?
C1 O1 Ca1 165.2(2) . . ?
C4 O4 Ca1 163.12(15) . . ?
C2 N1 C3 112.9(2) . . ?
C2 N1 H2 110.8(17) . . ?
C3 N1 H2 109.3(16) . . ?
C6 N2 C5 113.25(17) . . ?
C6 N2 H7 113.0(15) . . ?
C5 N2 H7 104.1(15) . . ?
C6 N2 H8 108(2) . . ?
C5 N2 H8 108(2) . . ?
H7 N2 H8 110(3) . . ?
O3 C4 O4 128.53(18) . . ?
O3 C4 C5 117.74(16) . . ?
O4 C4 C5 113.73(18) . . ?
O2 C1 O1 128.3(2) . . ?
O2 C1 C2 117.5(2) . . ?
O1 C1 C2 114.2(2) . . ?
N2 C5 C4 112.06(16) . . ?
N2 C5 H5 105.0(15) . . ?
C4 C5 H5 110.3(14) . . ?
N2 C5 H6 107.0(15) . . ?
C4 C5 H6 110.5(15) . . ?
H5 C5 H6 112(2) . . ?
N1 C2 C1 111.8(2) . . ?
N1 C2 H1 109.6(14) . . ?
C1 C2 H1 110.5(15) . . ?
N2 C6 H9 106.1(16) . . ?
N2 C6 H10 110.1(16) . . ?
H9 C6 H10 119(2) . . ?
N2 C6 H11 108(2) . . ?
H9 C6 H11 105(3) . . ?
H10 C6 H11 108(3) . . ?
N1 C3 H3 110.1(17) . . ?
N1 C3 H4 116(3) . . ?
H3 C3 H4 106(2) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H2 Br1 0.89(3) 2.43(3) 3.2864(12) 161(2) 7_565
N2 H7 Br1 0.96(3) 2.44(3) 3.3188(17) 152(2) 7_665
N2 H8 Br1 0.82(3) 2.55(3) 3.3287(18) 160(3) 3_656

_refine_diff_density_max         0.551
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.081

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC16
_database_code_depnum_ccdc_archive 'CCDC 1841212'
_audit_update_record             
;
2018-05-03 deposited with the CCDC.
2018-06-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C9 H25 Mg N3 O6, 2(Br)'
_chemical_formula_sum            'C9 H25 Br2 Mg N3 O8'
_chemical_formula_weight         487.45

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   9.5844(6)
_cell_length_b                   18.9445(13)
_cell_length_c                   9.9448(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1805.7(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    889
_cell_measurement_theta_min      2.0
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.793
_exptl_crystal_F_000             984
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    4.564
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.881
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
'The program SADABS-2008/1 - G.M. Sheldrick was used to apply a multi-scan absorption correction.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Tube'
_diffrn_measurement_device_type  'Rigaku Mercury2 (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 13.6612
_diffrn_reflns_number            17644
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_av_R_equivalents  0.0624
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.150
_diffrn_reflns_theta_max         27.506
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2139
_reflns_number_gt                1586
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2139
_refine_ls_number_parameters     166
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0288
_refine_ls_wR_factor_ref         0.1090
_refine_ls_wR_factor_gt          0.0868
_refine_ls_goodness_of_fit_ref   0.794
_refine_ls_restrained_S_all      0.794
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br -0.00726(3) 0.90724(2) 0.73364(3) 0.02228(15) Uani 1 1 d . . . . .
Mg1 Mg 0.41407(13) 0.7500 0.21872(13) 0.0114(3) Uani 1 2 d S T P . .
O3 O 0.3049(2) 0.66822(10) 0.1236(2) 0.0145(4) Uani 1 1 d . . . . .
O2 O 0.0461(3) 0.7500 0.4501(3) 0.0157(6) Uani 1 2 d S T P . .
O5 O 0.5240(2) 0.82748(12) 0.3227(2) 0.0154(4) Uani 1 1 d . . . . .
O4 O 0.4635(2) 0.58132(11) 0.1268(2) 0.0197(5) Uani 1 1 d . . . . .
O1 O 0.2560(3) 0.7500 0.3528(3) 0.0201(7) Uani 1 2 d S T P . .
N1 N 0.1418(4) 0.7500 0.7002(4) 0.0176(7) Uani 1 2 d S T P . .
N2 N 0.3080(3) 0.49127(14) -0.0116(3) 0.0173(6) Uani 1 1 d . . . . .
C1 C 0.1762(4) 0.7500 0.4523(4) 0.0128(8) Uani 1 2 d S T P . .
C4 C 0.3471(3) 0.60635(15) 0.0988(3) 0.0131(6) Uani 1 1 d . . . . .
C5 C 0.2410(3) 0.55744(17) 0.0342(3) 0.0166(6) Uani 1 1 d . . . . .
C2 C 0.2466(4) 0.7500 0.5905(4) 0.0172(9) Uani 1 2 d S T P . .
C6 C 0.2070(4) 0.43948(18) -0.0679(4) 0.0221(7) Uani 1 1 d . . . . .
C3 C 0.2062(6) 0.7500 0.8363(5) 0.0290(11) Uani 1 2 d S T P . .
H1 H 0.304(3) 0.7083(17) 0.597(3) 0.014(8) Uiso 1 1 d . . . . .
H2 H 0.085(4) 0.711(2) 0.696(4) 0.036(11) Uiso 1 1 d . . . . .
H3 H 0.266(4) 0.707(2) 0.847(4) 0.030(11) Uiso 1 1 d . . . . .
H4 H 0.131(7) 0.7500 0.902(7) 0.050(18) Uiso 1 2 d S . P . .
H5 H 0.193(4) 0.5761(17) -0.040(4) 0.015(8) Uiso 1 1 d . . . . .
H6 H 0.170(3) 0.5445(16) 0.100(3) 0.012(8) Uiso 1 1 d . . . . .
H7 H 0.368(4) 0.501(2) -0.069(5) 0.039(12) Uiso 1 1 d . . . . .
H8 H 0.348(4) 0.4715(19) 0.053(4) 0.024(10) Uiso 1 1 d . . . . .
H9 H 0.156(4) 0.4592(19) -0.138(4) 0.024(9) Uiso 1 1 d . . . . .
H10 H 0.137(4) 0.4279(17) 0.006(4) 0.020(9) Uiso 1 1 d . . . . .
H11 H 0.260(4) 0.398(2) -0.109(5) 0.045(13) Uiso 1 1 d . . . . .
H12 H 0.608(5) 0.819(2) 0.339(4) 0.046(13) Uiso 1 1 d . . . . .
H13 H 0.522(4) 0.863(3) 0.265(4) 0.026(11) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mg1 O1 2.019(3) . ?
Mg1 O5 2.082(2) 7_575 ?
Mg1 O5 2.082(2) . ?
Mg1 O3 2.096(2) 7_575 ?
Mg1 O3 2.096(2) . ?
Mg1 O2 2.102(3) 6_656 ?
Mg1 H13 2.41(5) . ?
O3 C4 1.264(3) . ?
O2 C1 1.248(5) . ?
O2 Mg1 2.102(3) 6_556 ?
O5 H12 0.84(5) . ?
O5 H13 0.88(5) . ?
O4 C4 1.244(3) . ?
O1 C1 1.250(5) . ?
N1 C2 1.483(6) . ?
N1 C3 1.487(6) . ?
N1 H2 0.92(4) . ?
N2 C5 1.480(4) . ?
N2 C6 1.488(4) . ?
N2 H7 0.83(4) . ?
N2 H8 0.84(4) . ?
C1 C2 1.531(6) . ?
C4 C5 1.518(4) . ?
C5 H5 0.94(3) . ?
C5 H6 0.97(3) . ?
C2 H1 0.96(3) . ?
C6 H9 0.93(4) . ?
C6 H10 1.02(4) . ?
C6 H11 1.01(5) . ?
C3 H3 1.01(4) . ?
C3 H4 0.98(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Mg1 O5 92.97(10) . 7_575 ?
O1 Mg1 O5 92.97(10) . . ?
O5 Mg1 O5 89.67(14) 7_575 . ?
O1 Mg1 O3 85.61(9) . 7_575 ?
O5 Mg1 O3 176.73(10) 7_575 7_575 ?
O5 Mg1 O3 87.47(8) . 7_575 ?
O1 Mg1 O3 85.61(9) . . ?
O5 Mg1 O3 87.47(8) 7_575 . ?
O5 Mg1 O3 176.73(10) . . ?
O3 Mg1 O3 95.35(12) 7_575 . ?
O1 Mg1 O2 168.37(14) . 6_656 ?
O5 Mg1 O2 95.27(9) 7_575 6_656 ?
O5 Mg1 O2 95.27(9) . 6_656 ?
O3 Mg1 O2 86.57(9) 7_575 6_656 ?
O3 Mg1 O2 86.57(9) . 6_656 ?
O1 Mg1 H13 101.3(9) . . ?
O5 Mg1 H13 108.3(11) 7_575 . ?
O5 Mg1 H13 21.0(10) . . ?
O3 Mg1 H13 69.2(11) 7_575 . ?
O3 Mg1 H13 162.3(10) . . ?
O2 Mg1 H13 83.9(9) 6_656 . ?
C4 O3 Mg1 127.85(18) . . ?
C1 O2 Mg1 128.0(3) . 6_556 ?
Mg1 O5 H12 117(3) . . ?
Mg1 O5 H13 101(3) . . ?
H12 O5 H13 107(4) . . ?
C1 O1 Mg1 169.1(3) . . ?
C2 N1 C3 112.8(4) . . ?
C2 N1 H2 112(3) . . ?
C3 N1 H2 107(3) . . ?
C5 N2 C6 113.1(3) . . ?
C5 N2 H7 108(3) . . ?
C6 N2 H7 110(3) . . ?
C5 N2 H8 110(2) . . ?
C6 N2 H8 107(3) . . ?
H7 N2 H8 108(4) . . ?
O2 C1 O1 126.7(4) . . ?
O2 C1 C2 117.2(4) . . ?
O1 C1 C2 116.2(3) . . ?
O4 C4 O3 126.6(3) . . ?
O4 C4 C5 117.6(3) . . ?
O3 C4 C5 115.7(2) . . ?
N2 C5 C4 110.9(2) . . ?
N2 C5 H5 107(2) . . ?
C4 C5 H5 116(2) . . ?
N2 C5 H6 107.1(19) . . ?
C4 C5 H6 109.7(19) . . ?
H5 C5 H6 106(3) . . ?
N1 C2 C1 111.2(3) . . ?
N1 C2 H1 110(2) . . ?
C1 C2 H1 108(2) . . ?
N2 C6 H9 111(2) . . ?
N2 C6 H10 107.3(19) . . ?
H9 C6 H10 107(3) . . ?
N2 C6 H11 109(2) . . ?
H9 C6 H11 106(3) . . ?
H10 C6 H11 117(3) . . ?
N1 C3 H3 109(2) . . ?
N1 C3 H4 107(4) . . ?
H3 C3 H4 111(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H2 Br1 0.92(4) 2.44(4) 3.3203(17) 161(3) 7_575
N2 H7 Br1 0.83(4) 2.67(4) 3.422(3) 152(4) 4_565
N2 H8 Br1 0.84(4) 2.65(4) 3.483(3) 171(3) 8_655

_refine_diff_density_max         0.386
_refine_diff_density_min         -0.750
_refine_diff_density_rms         0.106

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC17
_database_code_depnum_ccdc_archive 'CCDC 1841209'
_audit_update_record             
;
2018-05-03 deposited with the CCDC.
2018-06-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C9 H21 Ca0.57 N3 O6 Sr0.43, 2(Cl)'
_chemical_formula_sum            'C9 H21 Ca0.57 Cl2 N3 O6 Sr0.43'
_chemical_formula_weight         398.71

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sr Sr -1.5307 3.2498 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   8.9965(7)
_cell_length_b                   17.6045(3)
_cell_length_c                   10.3191(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1634.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    893
_cell_measurement_theta_min      2.0
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_F_000             823
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    1.992
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.672
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
'The program SADABS-2008/1 - G.M. Sheldrick was used to apply a multi-scan absorption correction.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Tube'
_diffrn_measurement_device_type  'Rigaku Mercury2 (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 13.6612
_diffrn_reflns_number            15958
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_av_R_equivalents  0.0732
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.288
_diffrn_reflns_theta_max         27.466
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             1926
_reflns_number_gt                1496
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1926
_refine_ls_number_parameters     150
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0522
_refine_ls_wR_factor_ref         0.1521
_refine_ls_wR_factor_gt          0.1460
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.079
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.53215(8) 0.7500 0.22769(6) 0.0241(3) Uani 0.566(7) 2 d S T P . .
Sr1 Sr 0.53215(8) 0.7500 0.22769(6) 0.0241(3) Uani 0.434(7) 2 d S T P . .
Cl2 Cl 0.99289(9) 0.91641(5) 0.71762(9) 0.0273(3) Uani 1 1 d . . . . .
O1 O 0.6628(6) 0.7500 0.4244(4) 0.0591(14) Uani 1 2 d S T P . .
O2 O 0.9024(5) 0.7500 0.4789(4) 0.0402(10) Uani 1 2 d S T P . .
C1 C 0.7692(7) 0.7500 0.5026(5) 0.0332(12) Uani 1 2 d S T P . .
C2 C 0.7218(6) 0.7500 0.6438(5) 0.0270(11) Uani 1 2 d S T P . .
N1 N 0.8492(5) 0.7500 0.7332(4) 0.0242(9) Uani 1 2 d S T P . .
C3 C 0.8018(7) 0.7500 0.8702(5) 0.0366(13) Uani 1 2 d S T P . .
O3 O 0.1387(4) 0.6355(2) 0.3697(3) 0.0650(11) Uani 1 1 d . . . . .
O4 O 0.3731(6) 0.6621(2) 0.3265(3) 0.0785(14) Uani 1 1 d . . . . .
C4 C 0.2734(6) 0.6238(2) 0.3741(3) 0.0390(10) Uani 1 1 d . . . . .
C5 C 0.3259(4) 0.5531(2) 0.4466(3) 0.0267(8) Uani 1 1 d . . . . .
N2 N 0.1986(3) 0.50755(17) 0.4959(3) 0.0265(7) Uani 1 1 d . . . . .
C6 C 0.2475(6) 0.4407(3) 0.5703(5) 0.0407(10) Uani 1 1 d . . . . .
H1 H 0.669(4) 0.706(2) 0.669(4) 0.030(10) Uiso 1 1 d . . . . .
H2 H 0.909(5) 0.709(2) 0.721(4) 0.041(12) Uiso 1 1 d . . . . .
H3 H 0.743(5) 0.704(3) 0.886(5) 0.052(13) Uiso 1 1 d . . . . .
H4 H 0.879(7) 0.7500 0.929(5) 0.028(14) Uiso 1 2 d S . P . .
H5 H 0.396(5) 0.564(2) 0.525(4) 0.040(11) Uiso 1 1 d . . . . .
H6 H 0.374(4) 0.522(2) 0.390(4) 0.026(10) Uiso 1 1 d . . . . .
H7 H 0.134(5) 0.540(2) 0.547(4) 0.034(10) Uiso 1 1 d . . . . .
H8 H 0.142(5) 0.494(2) 0.421(4) 0.030(10) Uiso 1 1 d . . . . .
H9 H 0.303(6) 0.456(3) 0.642(6) 0.060(16) Uiso 1 1 d . . . . .
H10 H 0.300(5) 0.411(3) 0.528(5) 0.045(15) Uiso 1 1 d . . . . .
H11 H 0.163(6) 0.414(3) 0.602(5) 0.055(15) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ca1 O4 2.341(3) 7_575 ?
Ca1 O4 2.341(3) . ?
Ca1 O1 2.346(4) . ?
Ca1 O2 2.430(4) 6_556 ?
Ca1 O3 2.448(3) 6_656 ?
Ca1 O3 2.448(3) 4_565 ?
Ca1 Sr1 4.5217(4) 6_556 ?
Ca1 Sr1 4.5218(4) 6_656 ?
O1 C1 1.252(7) . ?
O2 C1 1.223(7) . ?
O2 Sr1 2.431(4) 6_656 ?
O2 Ca1 2.431(4) 6_656 ?
C1 C2 1.518(7) . ?
C1 Sr1 3.353(6) 6_656 ?
C2 N1 1.471(6) . ?
C2 H1 0.95(4) . ?
N1 C3 1.477(7) . ?
N1 H2 0.92(4) . ?
C3 H3 0.98(5) . ?
C3 H4 0.92(6) . ?
O3 C4 1.230(6) . ?
O3 Sr1 2.449(3) 6_556 ?
O3 Ca1 2.449(3) 6_556 ?
O4 C4 1.225(6) . ?
C4 C5 1.528(5) . ?
C4 Sr1 3.279(4) 6_556 ?
C5 N2 1.487(5) . ?
C5 H5 1.04(5) . ?
C5 H6 0.90(4) . ?
N2 C6 1.473(5) . ?
N2 H7 0.97(4) . ?
N2 H8 0.95(4) . ?
C6 H9 0.93(6) . ?
C6 H10 0.83(5) . ?
C6 H11 0.96(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Ca1 O4 82.7(2) 7_575 . ?
O4 Ca1 O1 85.93(15) 7_575 . ?
O4 Ca1 O1 85.93(15) . . ?
O4 Ca1 O2 95.09(13) 7_575 6_556 ?
O4 Ca1 O2 95.09(13) . 6_556 ?
O1 Ca1 O2 178.64(18) . 6_556 ?
O4 Ca1 O3 164.24(17) 7_575 6_656 ?
O4 Ca1 O3 82.76(15) . 6_656 ?
O1 Ca1 O3 99.16(11) . 6_656 ?
O2 Ca1 O3 80.09(10) 6_556 6_656 ?
O4 Ca1 O3 82.76(15) 7_575 4_565 ?
O4 Ca1 O3 164.24(17) . 4_565 ?
O1 Ca1 O3 99.16(11) . 4_565 ?
O2 Ca1 O3 80.09(10) 6_556 4_565 ?
O3 Ca1 O3 110.9(2) 6_656 4_565 ?
O4 Ca1 Sr1 49.29(13) 7_575 6_556 ?
O4 Ca1 Sr1 49.29(13) . 6_556 ?
O1 Ca1 Sr1 114.22(14) . 6_556 ?
O2 Ca1 Sr1 67.14(11) 6_556 6_556 ?
O3 Ca1 Sr1 115.56(10) 6_656 6_556 ?
O3 Ca1 Sr1 115.56(10) 4_565 6_556 ?
O4 Ca1 Sr1 124.30(13) 7_575 6_656 ?
O4 Ca1 Sr1 124.30(13) . 6_656 ?
O1 Ca1 Sr1 54.09(14) . 6_656 ?
O2 Ca1 Sr1 124.54(11) 6_556 6_656 ?
O3 Ca1 Sr1 69.65(10) 6_656 6_656 ?
O3 Ca1 Sr1 69.65(10) 4_565 6_656 ?
Sr1 Ca1 Sr1 168.31(3) 6_556 6_656 ?
C1 O1 Ca1 160.2(5) . . ?
C1 O2 Sr1 130.3(4) . 6_656 ?
C1 O2 Ca1 130.3(4) . 6_656 ?
Sr1 O2 Ca1 0.0 6_656 6_656 ?
O2 C1 O1 128.3(5) . . ?
O2 C1 C2 117.9(5) . . ?
O1 C1 C2 113.8(5) . . ?
O2 C1 Sr1 33.6(3) . 6_656 ?
O1 C1 Sr1 94.7(4) . 6_656 ?
C2 C1 Sr1 151.5(4) . 6_656 ?
N1 C2 C1 112.5(4) . . ?
N1 C2 H1 103(2) . . ?
C1 C2 H1 114(2) . . ?
C2 N1 C3 112.0(4) . . ?
C2 N1 H2 112(3) . . ?
C3 N1 H2 108(3) . . ?
N1 C3 H3 108(3) . . ?
N1 C3 H4 114(4) . . ?
H3 C3 H4 107(3) . . ?
C4 O3 Sr1 122.6(3) . 6_556 ?
C4 O3 Ca1 122.6(3) . 6_556 ?
Sr1 O3 Ca1 0.0 6_556 6_556 ?
C4 O4 Ca1 170.4(4) . . ?
O4 C4 O3 127.9(4) . . ?
O4 C4 C5 114.7(5) . . ?
O3 C4 C5 117.3(4) . . ?
O4 C4 Sr1 89.1(3) . 6_556 ?
O3 C4 Sr1 39.0(2) . 6_556 ?
C5 C4 Sr1 156.1(3) . 6_556 ?
N2 C5 C4 111.6(3) . . ?
N2 C5 H5 107(2) . . ?
C4 C5 H5 115(2) . . ?
N2 C5 H6 106(2) . . ?
C4 C5 H6 109(2) . . ?
H5 C5 H6 108(3) . . ?
C6 N2 C5 112.3(3) . . ?
C6 N2 H7 112(2) . . ?
C5 N2 H7 109(2) . . ?
C6 N2 H8 112(2) . . ?
C5 N2 H8 106(2) . . ?
H7 N2 H8 106(3) . . ?
N2 C6 H9 110(4) . . ?
N2 C6 H10 113(4) . . ?
H9 C6 H10 108(5) . . ?
N2 C6 H11 110(3) . . ?
H9 C6 H11 107(4) . . ?
H10 C6 H11 109(5) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H2 Cl2 0.92(4) 2.33(4) 3.206(2) 161(4) 7_575
N2 H7 Cl2 0.97(4) 2.31(4) 3.233(3) 160(3) 7_475
N2 H8 Cl2 0.95(4) 2.32(4) 3.224(3) 158(3) 3_646

_refine_diff_density_max         1.207
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.099

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC18
_database_code_depnum_ccdc_archive 'CCDC 1841214'
_audit_update_record             
;
2018-05-03 deposited with the CCDC.
2018-06-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C9 H25 Mn N3 O8, 2(I)'
_chemical_formula_sum            'C9 H25 I2 Mn N3 O8'
_chemical_formula_weight         612.06

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   9.8288(7)
_cell_length_b                   19.2160(15)
_cell_length_c                   10.2845(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1942.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    871
_cell_measurement_theta_min      2.0
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.093
_exptl_crystal_F_000             1180
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    3.896
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.665
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
'The program SADABS-2008/1 - G.M. Sheldrick was used to apply a multi-scan absorption correction.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Tube'
_diffrn_measurement_device_type  'Rigaku Mercury2 (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 13.6612
_diffrn_reflns_number            18998
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_av_R_equivalents  0.0992
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.120
_diffrn_reflns_theta_max         27.524
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2301
_reflns_number_gt                1482
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0585P)²+7.7627P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2301
_refine_ls_number_parameters     147
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0406
_refine_ls_wR_factor_ref         0.1149
_refine_ls_wR_factor_gt          0.0947
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_restrained_S_all      0.978
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.01811(4) 0.40828(2) 0.74741(4) 0.02636(15) Uani 1 1 d . . . . .
Mn2 Mn 0.40815(12) 0.7500 0.78540(12) 0.0141(3) Uani 1 2 d S T P . .
O5 O 0.5201(4) 0.6681(2) 0.6794(4) 0.0186(9) Uani 1 1 d D . . . .
O2 O 0.0421(6) 0.7500 0.5442(6) 0.0209(13) Uani 1 2 d S T P . .
O3 O 0.2960(4) 0.6639(2) 0.8769(4) 0.0176(9) Uani 1 1 d . . . . .
O1 O 0.2416(6) 0.7500 0.6491(6) 0.0240(14) Uani 1 2 d S T P . .
C4 C 0.3424(6) 0.6042(3) 0.9040(5) 0.0162(12) Uani 1 1 d . . . . .
C1 C 0.1702(9) 0.7500 0.5492(8) 0.0162(17) Uani 1 2 d S T P . .
C2 C 0.2448(9) 0.7500 0.4193(8) 0.0193(18) Uani 1 2 d S T P . .
N1 N 0.1485(8) 0.7500 0.3091(7) 0.0205(16) Uani 1 2 d DS T P . .
O4 O 0.4580(4) 0.5819(2) 0.8790(4) 0.0230(10) Uani 1 1 d . . . . .
C5 C 0.2427(6) 0.5547(3) 0.9688(6) 0.0177(12) Uani 1 1 d . . . . .
H5 H 0.2023 0.5773 1.0438 0.021 Uiso 1 1 calc R U . . .
H6 H 0.1702 0.5434 0.9083 0.021 Uiso 1 1 calc R U . . .
N2 N 0.3110(6) 0.4895(3) 1.0109(5) 0.0190(11) Uani 1 1 d D . . . .
C6 C 0.2176(7) 0.4400(3) 1.0768(6) 0.0228(14) Uani 1 1 d . . . . .
H9 H 0.1763 0.4624 1.1503 0.034 Uiso 1 1 calc R U . . .
H11 H 0.2680 0.4001 1.1057 0.034 Uiso 1 1 calc R U . . .
H10 H 0.1481 0.4255 1.0171 0.034 Uiso 1 1 calc R U . . .
C3 C 0.2135(13) 0.7500 0.1783(10) 0.028(2) Uani 1 2 d S T P . .
H1 H 0.293(8) 0.711(3) 0.409(7) 0.03(2) Uiso 1 1 d . . . . .
H2 H 0.080(5) 0.714(3) 0.306(7) 0.04(2) Uiso 1 1 d D . . . .
H3 H 0.270(7) 0.712(4) 0.178(7) 0.03(2) Uiso 1 1 d . . . . .
H4 H 0.157(13) 0.7500 0.133(12) 0.04(4) Uiso 1 2 d S . P . .
H7 H 0.383(5) 0.503(4) 1.070(6) 0.03(2) Uiso 1 1 d D . . . .
H8 H 0.350(8) 0.469(4) 0.933(5) 0.05(3) Uiso 1 1 d D . . . .
H12 H 0.511(9) 0.630(3) 0.741(7) 0.07(3) Uiso 1 1 d D . . . .
H13 H 0.614(3) 0.671(4) 0.650(8) 0.06(3) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn2 O1 2.155(6) . ?
Mn2 O2 2.192(6) 6_657 ?
Mn2 O3 2.200(4) 8_575 ?
Mn2 O3 2.200(4) . ?
Mn2 O5 2.208(4) 8_575 ?
Mn2 O5 2.208(4) . ?
O2 C1 1.260(10) . ?
O2 Mn2 2.192(6) 6_557 ?
O3 C4 1.266(7) . ?
O1 C1 1.245(10) . ?
C4 O4 1.241(7) . ?
C4 C5 1.520(8) . ?
C1 C2 1.524(12) . ?
C2 N1 1.476(11) . ?
N1 C3 1.489(12) . ?
C5 N2 1.486(7) . ?
N2 C6 1.486(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Mn2 O2 167.5(2) . 6_657 ?
O1 Mn2 O3 84.12(16) . 8_575 ?
O2 Mn2 O3 87.66(15) 6_657 8_575 ?
O1 Mn2 O3 84.12(16) . . ?
O2 Mn2 O3 87.66(15) 6_657 . ?
O3 Mn2 O3 97.5(2) 8_575 . ?
O1 Mn2 O5 93.30(17) . 8_575 ?
O2 Mn2 O5 95.46(16) 6_657 8_575 ?
O3 Mn2 O5 85.70(15) 8_575 8_575 ?
O3 Mn2 O5 175.60(16) . 8_575 ?
O1 Mn2 O5 93.30(17) . . ?
O2 Mn2 O5 95.46(16) 6_657 . ?
O3 Mn2 O5 175.60(16) 8_575 . ?
O3 Mn2 O5 85.70(15) . . ?
O5 Mn2 O5 90.9(2) 8_575 . ?
C1 O2 Mn2 124.6(6) . 6_557 ?
C4 O3 Mn2 126.5(4) . . ?
C1 O1 Mn2 164.9(6) . . ?
O4 C4 O3 126.7(5) . . ?
O4 C4 C5 117.6(5) . . ?
O3 C4 C5 115.6(5) . . ?
O1 C1 O2 126.7(8) . . ?
O1 C1 C2 116.9(7) . . ?
O2 C1 C2 116.4(8) . . ?
N1 C2 C1 111.3(7) . . ?
C2 N1 C3 114.7(8) . . ?
N2 C5 C4 111.4(5) . . ?
C6 N2 C5 113.1(5) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H2 I1 0.96(2) 2.61(4) 3.503(4) 155(6) 5_566
N2 H8 I1 0.97(2) 2.75(3) 3.692(5) 165(7) 6_657
N2 H7 I1 0.96(2) 2.69(4) 3.549(5) 149(6) 2_565

_refine_diff_density_max         1.479
_refine_diff_density_min         -1.112
_refine_diff_density_rms         0.178

