# 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_18_pjs040_Hyd2CoCl4
_database_code_depnum_ccdc_archive 'CCDC 1877363'
_audit_update_record             
;
2018-11-06 deposited with the CCDC.
2018-12-27 downloaded from the CCDC.
;
_audit_creation_date             2018-02-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3461 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cl2 Co H14 N4 O2, 2(Cl)'
_chemical_formula_sum            'Cl4 Co H14 N4 O2'
_chemical_formula_weight         302.88
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   7.9880(6)
_cell_length_b                   5.7019(5)
_cell_length_c                   11.3808(8)
_cell_angle_alpha                90
_cell_angle_beta                 97.745(7)
_cell_angle_gamma                90
_cell_volume                     513.63(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1105
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.9940
_cell_measurement_theta_min      4.0100
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.677
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93868
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.958
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       blade
_exptl_crystal_F_000             306
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0513
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.867
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2489
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.867
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.487
_diffrn_reflns_theta_min         3.613
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2887
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.867
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -20.00  28.00   1.00   11.83    --  -10.46 -99.00 -30.00   48
  2  ω    -39.00  13.00   1.00   11.83    --  -10.46 -38.00   0.00   52
  3  ω    -36.00  52.00   1.00   11.83    --   11.79 -19.00 150.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0891536000
_diffrn_orient_matrix_UB_12      0.0077140000
_diffrn_orient_matrix_UB_13      0.0034795000
_diffrn_orient_matrix_UB_21      0.0072269000
_diffrn_orient_matrix_UB_22      -0.1195771000
_diffrn_orient_matrix_UB_23      0.0171891000
_diffrn_orient_matrix_UB_31      -0.0053242000
_diffrn_orient_matrix_UB_32      -0.0335763000
_diffrn_orient_matrix_UB_33      -0.0603818000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1053
_reflns_number_total             1236
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.118
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     54
_refine_ls_number_reflns         1236
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0311
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0169P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0548
_refine_ls_wR_factor_ref         0.0602
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O1(H1A,H1B)
2.b Secondary CH2 refined with riding coordinates:
 N1(H1C,H1D)
2.c Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
Co1 Co 0.5000 0.5000 0.5000 0.01496(14) Uani 1 2 d S T P . .
Cl1 Cl 0.49196(8) 0.80918(12) 0.35553(5) 0.02075(16) Uani 1 1 d . . . . .
Cl2 Cl 0.96251(8) 0.68534(13) 0.35875(5) 0.02540(18) Uani 1 1 d . . . . .
O1 O 0.3128(2) 0.6845(3) 0.58206(14) 0.0224(4) Uani 1 1 d . . . . .
H1A H 0.3562 0.7425 0.6503 0.034 Uiso 1 1 d GR . . . .
H1B H 0.2368 0.5872 0.6010 0.034 Uiso 1 1 d GR . . . .
N1 N 0.7067(3) 0.6554(4) 0.61726(15) 0.0195(5) Uani 1 1 d . . . . .
H1C H 0.6658 0.6956 0.6834 0.023 Uiso 1 1 calc R . . . .
H1D H 0.7819 0.5420 0.6369 0.023 Uiso 1 1 calc R . . . .
N2 N 0.7992(3) 0.8555(4) 0.58221(17) 0.0236(5) Uani 1 1 d . . . . .
H2A H 0.8507 0.8172 0.5203 0.028 Uiso 1 1 calc GR . . . .
H2B H 0.8759 0.8991 0.6423 0.028 Uiso 1 1 calc GR . . . .
H2C H 0.7280 0.9735 0.5625 0.028 Uiso 1 1 calc GR . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.0153(3) 0.0148(3) 0.0144(2) 0.00040(19) 0.00061(17) -0.0010(2)
Cl1 0.0254(4) 0.0194(4) 0.0179(3) 0.0028(2) 0.0046(2) 0.0013(3)
Cl2 0.0235(4) 0.0292(4) 0.0235(3) 0.0009(3) 0.0028(2) 0.0006(3)
O1 0.0226(10) 0.0235(11) 0.0209(8) -0.0058(8) 0.0024(7) -0.0035(8)
N1 0.0199(11) 0.0201(13) 0.0182(9) 0.0000(9) 0.0014(8) -0.0007(10)
N2 0.0210(12) 0.0221(14) 0.0280(11) -0.0034(10) 0.0041(9) -0.0036(10)

_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
Co1 Cl1 2.4056(6) 3_666 ?
Co1 Cl1 2.4056(6) . ?
Co1 O1 2.1430(18) . ?
Co1 O1 2.1430(18) 3_666 ?
Co1 N1 2.1675(19) 3_666 ?
Co1 N1 2.1675(19) . ?
O1 H1A 0.8717 . ?
O1 H1B 0.8708 . ?
N1 H1C 0.8900 . ?
N1 H1D 0.8900 . ?
N1 N2 1.445(3) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?

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
Cl1 Co1 Cl1 180.00(3) . 3_666 ?
O1 Co1 Cl1 91.02(5) . 3_666 ?
O1 Co1 Cl1 88.98(5) . . ?
O1 Co1 Cl1 91.02(5) 3_666 . ?
O1 Co1 Cl1 88.98(5) 3_666 3_666 ?
O1 Co1 O1 180.0 . 3_666 ?
O1 Co1 N1 92.83(7) 3_666 3_666 ?
O1 Co1 N1 87.17(7) 3_666 . ?
O1 Co1 N1 92.83(7) . . ?
O1 Co1 N1 87.17(7) . 3_666 ?
N1 Co1 Cl1 86.03(6) . 3_666 ?
N1 Co1 Cl1 93.97(6) . . ?
N1 Co1 Cl1 86.03(6) 3_666 . ?
N1 Co1 Cl1 93.97(6) 3_666 3_666 ?
N1 Co1 N1 180.0 . 3_666 ?
Co1 O1 H1A 110.9 . . ?
Co1 O1 H1B 110.2 . . ?
H1A O1 H1B 103.2 . . ?
Co1 N1 H1C 106.9 . . ?
Co1 N1 H1D 106.9 . . ?
H1C N1 H1D 106.7 . . ?
N2 N1 Co1 121.90(13) . . ?
N2 N1 H1C 106.9 . . ?
N2 N1 H1D 106.9 . . ?
N1 N2 H2A 109.5 . . ?
N1 N2 H2B 109.5 . . ?
N1 N2 H2C 109.5 . . ?
H2A N2 H2B 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?

_iucr_refine_instructions_details 
;

    18_pjs040.res created by SHELXL-2014/7

TITL 18_pjs040_a.res in P2(1)/c
REM Old TITL 18_PJS040 in P21/c #14
REM SHELXT solution in P2(1)/c
REM R1 0.086, Rweak 0.003, Alpha 0.017, Orientation as input
REM Formula found by SHELXT: N6 Mn Cl4
CELL 0.71073 7.987998 5.70189 11.380785 90 97.7453 90
ZERR 2 0.000643 0.000489 0.000798 0 0.0069 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC Cl Co H N O
UNIT 8 2 28 8 4
 
L.S. 10
PLAN  20
BOND $H
LIST 6
MORE -1
CONF
fmap 2
acta 52
REM <olex2.extras>
REM <HklSrc "%./18_PJS040.hkl">
REM </olex2.extras>
 
WGHT    0.016900
FVAR       0.77577
CO1   2    0.500000    0.500000    0.500000    10.50000    0.01529    0.01485 =
         0.01436    0.00040    0.00061   -0.00102
CL1   1    0.491962    0.809178    0.355531    11.00000    0.02542    0.01939 =
         0.01790    0.00283    0.00460    0.00130
CL2   1    0.962513    0.685340    0.358745    11.00000    0.02345    0.02919 =
         0.02346    0.00094    0.00281    0.00056
O1    5    0.312786    0.684544    0.582064    11.00000    0.02262    0.02354 =
         0.02091   -0.00583    0.00242   -0.00348
AFIX   7
H1A   3    0.356186    0.742454    0.650304    11.00000   -1.50000
H1B   3    0.236776    0.587184    0.600964    11.00000   -1.50000
AFIX   0
N1    4    0.706690    0.655393    0.617261    11.00000    0.01989    0.02009 =
         0.01817   -0.00004    0.00141   -0.00071
AFIX  23
H1C   3    0.665778    0.695609    0.683390    11.00000   -1.20000
H1D   3    0.781861    0.542038    0.636901    11.00000   -1.20000
AFIX   0
N2    4    0.799223    0.855487    0.582206    11.00000    0.02096    0.02206 =
         0.02800   -0.00341    0.00412   -0.00358
AFIX 137
H2A   3    0.850726    0.817189    0.520262    11.00000   -1.20000
H2B   3    0.875937    0.899088    0.642301    11.00000   -1.20000
H2C   3    0.728018    0.973465    0.562457    11.00000   -1.20000
AFIX   0
HKLF 4
 
REM  18_pjs040_a.res in P2(1)/c
REM R1 =  0.0311 for    1053 Fo > 4sig(Fo)  and  0.0429 for all    1236 data
REM     54 parameters refined using      0 restraints
 
END  
     
WGHT      0.0169      0.0000 

REM Highest difference peak  0.439,  deepest hole -0.429,  1-sigma level  0.118
Q1    1   0.3574  0.7945  0.2781  11.00000  0.05    0.44
Q2    1   1.0766  0.6660  0.4555  11.00000  0.05    0.44
Q3    1   0.3716  0.8848  0.3657  11.00000  0.05    0.41
Q4    1   1.0111  0.6981  0.3191  11.00000  0.05    0.41
Q5    1   0.2538  0.4882  0.5358  11.00000  0.05    0.39
Q6    1   0.7292  1.1561  0.6532  11.00000  0.05    0.38
Q7    1   1.0000  0.5000  0.5000  10.50000  0.05    0.37
Q8    1   1.1026  0.7062  0.2620  11.00000  0.05    0.37
Q9    1   0.0137  0.6074  0.5804  11.00000  0.05    0.37
Q10   1   0.9565  1.0012  0.7239  11.00000  0.05    0.36
Q11   1   0.8890  0.6146  0.6045  11.00000  0.05    0.36
Q12   1   0.8649  0.4960  0.2869  11.00000  0.05    0.34
Q13   1   0.3972  0.6420  0.4659  11.00000  0.05    0.34
Q14   1   0.5868  0.9973  0.3373  11.00000  0.05    0.33
Q15   1   0.6684  0.7840  0.7401  11.00000  0.05    0.33
Q16   1   0.9350  0.6847  0.4527  11.00000  0.05    0.33
Q17   1   0.8376  0.8562  0.4170  11.00000  0.05    0.32
Q18   1   0.5040  0.9657  0.4598  11.00000  0.05    0.32
Q19   1   0.3062  1.0090  0.6765  11.00000  0.05    0.32
Q20   1   1.0625  0.6065  0.4040  11.00000  0.05    0.32

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0311 for 1053 Fo > 4sig(Fo) and 0.0429 for all 2678 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.44, deepest hole -0.43
  REM Mean Shift 0, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0429
  REM R1_gt = 0.0311
  REM wR_ref = 0.0602
  REM GOOF = 1.050
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 2678
  REM Reflections_gt = 1053
  REM Parameters = n/a
  REM Hole = -0.43
  REM Peak = 0.44
  REM Flack = n/a

  
;
_olex2_date_sample_data_collection 2018-01-18
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.062
_oxdiff_exptl_absorpt_empirical_full_min 0.938
####################################################################### 
# 
# 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_18_pjs041_Hyd10MnCl16
_database_code_depnum_ccdc_archive 'CCDC 1877366'
_audit_update_record             
;
2018-11-06 deposited with the CCDC.
2018-12-27 downloaded from the CCDC.
;
_audit_creation_date             2018-11-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cl6 Mn, 2(Cl4 H7 Mn N2 O), 2(Cl), 8(H5 N2)'
_chemical_formula_sum            'Cl16 H54 Mn3 N20 O2'
_chemical_formula_weight         1098.65
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Cl Mn N O'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.3639 0.7018 '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'
Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.5839(3)
_cell_length_b                   9.1752(4)
_cell_length_c                   15.0656(6)
_cell_angle_alpha                89.821(4)
_cell_angle_beta                 84.447(3)
_cell_angle_gamma                75.697(4)
_cell_volume                     1010.83(7)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    4133
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.8570
_cell_measurement_theta_min      4.9510
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    17.584
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34674
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.805
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             557
_exptl_crystal_size_max          0.179
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.070
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6591
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        68.000
_diffrn_reflns_theta_max         72.958
_diffrn_reflns_theta_min         4.975
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2887
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -26.00  35.00   1.00    1.00    --   41.91 -38.00 150.00   61
  2  ω      3.00  53.00   1.00    1.00    --   41.91 -99.00 120.00   50
  3  ω     40.00  87.00   1.00    1.06    --  105.91 -94.00  30.00   47
  4  ω     45.00 116.00   1.00    1.06    --  105.91-125.00 -60.00   71
  5  ω     57.00  96.00   1.00    1.00    --   41.91-125.00-150.00   39
  6  ω     53.00 124.00   1.00    1.06    --  105.91 -45.00-120.00   71
  7  ω     81.00 178.00   1.00    1.06    --  105.91  45.00 -60.00   97
  8  ω    150.00 176.00   1.00    1.06    --  105.91 125.00  90.00   26
  9  ω    106.00 142.00   1.00    1.06    --  105.91 125.00-120.00   36
 10  ω     35.00 142.00   1.00    1.06    --  105.91 -15.00 -60.00  107
 11  ω     44.00 114.00   1.00    1.06    --  105.91-125.00 120.00   70
 12  ω     42.00 131.00   1.00    1.06    --  105.91 -30.00 120.00   89
 13  ω     37.00 121.00   1.00    1.06    --  105.91 -77.00 120.00   84
 14  ω   -111.00 -10.00   1.00    1.00    --  -41.91 -77.00   0.00  101
 15  ω   -113.00 -25.00   1.00    1.00    --  -41.91 -38.00-120.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0397005000
_diffrn_orient_matrix_UB_12      -0.1434958000
_diffrn_orient_matrix_UB_13      0.0417246000
_diffrn_orient_matrix_UB_21      -0.0829945000
_diffrn_orient_matrix_UB_22      0.0891190000
_diffrn_orient_matrix_UB_23      0.0869433000
_diffrn_orient_matrix_UB_31      -0.1895199000
_diffrn_orient_matrix_UB_32      0.0387957000
_diffrn_orient_matrix_UB_33      -0.0354980000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3644
_reflns_number_total             3911
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.535
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         3911
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0316
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0377P)²+0.4995P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0818
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 N3-H3A = N3-H3B = N7-H7A = N7-H7B = N10-H10A = N10-H10B
 0.89 with sigma of 0.001
 H3A-H3B = H7A-H7B = H10A-H10B
 1.428 with sigma of 0.002
3.a Rotating group:
 O1(H1A,H1B), N5(H5A,H5B)
3.b Secondary CH2 refined with riding coordinates:
 N1(H1C,H1D)
3.c Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C), N9(H9A,H9B,H9C), N8(H8A,H8B,H8C), N4(H4A,H4B,H4C), N6(H6A,
 H6B,H6C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 -0.5000 0.5000 0.5000 0.01648(13) Uani 1 2 d S T P . .
Mn2 Mn 0.95130(5) 0.05312(4) 0.18877(2) 0.01648(11) Uani 1 1 d . . . . .
Cl3 Cl -0.24938(8) 0.55843(7) 0.38926(4) 0.02324(14) Uani 1 1 d . . . . .
Cl2 Cl -0.29886(8) 0.49457(7) 0.62936(4) 0.02346(14) Uani 1 1 d . . . . .
Cl1 Cl -0.64574(9) 0.78090(7) 0.52372(4) 0.02391(14) Uani 1 1 d . . . . .
Cl5 Cl 1.24024(8) -0.09464(7) 0.10203(4) 0.02515(15) Uani 1 1 d . . . . .
Cl7 Cl 0.75148(9) -0.09865(7) 0.13467(4) 0.02544(14) Uani 1 1 d . . . . .
Cl4 Cl 1.11015(8) 0.23635(7) 0.24905(4) 0.02193(14) Uani 1 1 d . . . . .
Cl6 Cl 1.00358(9) -0.10841(7) 0.32412(4) 0.02446(14) Uani 1 1 d . . . . .
Cl8 Cl 0.64950(11) 0.51942(8) 0.12642(5) 0.03888(18) Uani 1 1 d . . . . .
O1 O 0.9111(3) 0.2065(2) 0.06946(12) 0.0280(4) Uani 1 1 d . . . . .
H1A H 0.8270 0.2917 0.0834 0.042 Uiso 1 1 d GR . . . .
H1B H 0.8744 0.1631 0.0242 0.042 Uiso 1 1 d GR . . . .
N1 N 0.7054(3) 0.2257(2) 0.26166(14) 0.0190(4) Uani 1 1 d . . . . .
H1C H 0.7258 0.2273 0.3188 0.023 Uiso 1 1 calc R . . . .
H1D H 0.7089 0.3157 0.2404 0.023 Uiso 1 1 calc R . . . .
N2 N 0.5207(3) 0.2121(3) 0.25955(15) 0.0252(5) Uani 1 1 d . . . . .
H2A H 0.4924 0.2174 0.2035 0.030 Uiso 1 1 calc GR . . . .
H2B H 0.4444 0.2865 0.2921 0.030 Uiso 1 1 calc GR . . . .
H2C H 0.5112 0.1242 0.2818 0.030 Uiso 1 1 calc GR . . . .
N9 N -0.0538(3) 0.7220(3) 0.52623(16) 0.0274(5) Uani 1 1 d . . . . .
H9A H -0.0871 0.6738 0.4821 0.033 Uiso 1 1 calc GR . . . .
H9B H -0.0634 0.6725 0.5767 0.033 Uiso 1 1 calc GR . . . .
H9C H 0.0616 0.7271 0.5135 0.033 Uiso 1 1 calc GR . . . .
N8 N 0.0050(3) 0.5866(3) 0.21779(15) 0.0263(5) Uani 1 1 d . . . . .
H8A H -0.0966 0.6033 0.1902 0.032 Uiso 1 1 calc GR . . . .
H8B H -0.0003 0.6642 0.2541 0.032 Uiso 1 1 calc GR . . . .
H8C H 0.0153 0.5032 0.2493 0.032 Uiso 1 1 calc GR . . . .
N4 N 0.4559(4) -0.1902(3) 0.29335(19) 0.0372(6) Uani 1 1 d . . . . .
H4A H 0.4946 -0.1925 0.2356 0.045 Uiso 1 1 calc GR . . . .
H4B H 0.3343 -0.1690 0.3001 0.045 Uiso 1 1 calc GR . . . .
H4C H 0.5010 -0.2795 0.3165 0.045 Uiso 1 1 calc GR . . . .
N7 N 0.1608(4) 0.5689(3) 0.15266(19) 0.0396(6) Uani 1 1 d D . . . .
H7A H 0.261(2) 0.553(3) 0.1811(18) 0.048 Uiso 1 1 d D . . . .
H7B H 0.147(4) 0.6592(16) 0.1285(19) 0.048 Uiso 1 1 d D . . . .
N6 N 0.2745(4) 0.2821(3) 0.04183(16) 0.0391(6) Uani 1 1 d . . . . .
H6A H 0.2933 0.3128 -0.0136 0.047 Uiso 1 1 calc GR . . . .
H6B H 0.2225 0.3613 0.0775 0.047 Uiso 1 1 calc GR . . . .
H6C H 0.2011 0.2197 0.0427 0.047 Uiso 1 1 calc GR . . . .
N10 N -0.1693(5) 0.8696(3) 0.53659(19) 0.0468(8) Uani 1 1 d D . . . .
H10A H -0.154(5) 0.918(3) 0.4863(9) 0.056 Uiso 1 1 d D . . . .
H10B H -0.122(4) 0.913(3) 0.5783(12) 0.056 Uiso 1 1 d D . . . .
N3 N 0.5174(4) -0.0759(4) 0.33871(18) 0.0435(7) Uani 1 1 d D . . . .
H3A H 0.6338(14) -0.123(4) 0.3434(18) 0.052 Uiso 1 1 d D . . . .
H3B H 0.462(3) -0.063(4) 0.3939(7) 0.052 Uiso 1 1 d D . . . .
N5 N 0.4412(4) 0.2074(5) 0.07143(19) 0.0562(10) Uani 1 1 d . . . . .
H5A H 0.4284 0.1256 0.0962 0.067 Uiso 1 1 d GR . . . .
H5B H 0.5236 0.1863 0.0268 0.067 Uiso 1 1 d GR . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mn1 0.0181(3) 0.0174(3) 0.0132(2) 0.0011(2) 0.0005(2) -0.0038(2)
Mn2 0.0187(2) 0.0165(2) 0.01465(19) -0.00010(14) 0.00012(15) -0.00573(15)
Cl3 0.0207(3) 0.0286(3) 0.0200(3) 0.0033(2) 0.0033(2) -0.0074(2)
Cl2 0.0257(3) 0.0242(3) 0.0208(3) -0.0015(2) -0.0071(2) -0.0050(2)
Cl1 0.0308(3) 0.0190(3) 0.0195(3) 0.0011(2) 0.0017(2) -0.0031(2)
Cl5 0.0234(3) 0.0294(3) 0.0207(3) -0.0040(2) 0.0048(2) -0.0056(2)
Cl7 0.0303(3) 0.0276(3) 0.0224(3) -0.0020(2) -0.0047(2) -0.0140(3)
Cl4 0.0238(3) 0.0234(3) 0.0216(3) -0.0024(2) -0.0020(2) -0.0117(2)
Cl6 0.0348(3) 0.0221(3) 0.0167(3) 0.0043(2) -0.0030(2) -0.0074(3)
Cl8 0.0500(5) 0.0279(4) 0.0404(4) 0.0090(3) -0.0115(3) -0.0100(3)
O1 0.0386(11) 0.0267(10) 0.0188(9) 0.0015(7) -0.0078(8) -0.0066(8)
N1 0.0205(11) 0.0215(11) 0.0161(10) -0.0011(8) -0.0009(8) -0.0075(9)
N2 0.0200(11) 0.0268(12) 0.0271(11) -0.0057(9) 0.0005(9) -0.0037(9)
N9 0.0270(12) 0.0257(12) 0.0296(12) 0.0029(10) -0.0037(10) -0.0063(10)
N8 0.0311(12) 0.0247(12) 0.0218(11) -0.0005(9) -0.0015(9) -0.0050(10)
N4 0.0336(14) 0.0392(15) 0.0405(15) 0.0157(12) -0.0053(12) -0.0119(12)
N7 0.0502(17) 0.0293(14) 0.0381(15) -0.0021(11) 0.0173(13) -0.0156(12)
N6 0.0488(16) 0.0490(16) 0.0208(12) -0.0036(11) -0.0066(11) -0.0132(13)
N10 0.0596(19) 0.0374(16) 0.0301(14) 0.0022(12) 0.0026(13) 0.0103(14)
N3 0.0547(18) 0.0462(17) 0.0292(13) 0.0051(12) 0.0054(13) -0.0159(14)
N5 0.0293(15) 0.100(3) 0.0278(14) -0.0097(16) 0.0029(12) 0.0037(16)

_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 Cl3 2.5627(6) . ?
Mn1 Cl3 2.5627(6) 2_466 ?
Mn1 Cl2 2.5816(6) . ?
Mn1 Cl2 2.5817(6) 2_466 ?
Mn1 Cl1 2.5522(6) 2_466 ?
Mn1 Cl1 2.5522(6) . ?
Mn2 Cl5 2.5172(7) . ?
Mn2 Cl7 2.4877(7) . ?
Mn2 Cl4 2.5149(7) . ?
Mn2 Cl6 2.5217(7) . ?
Mn2 O1 2.2764(18) . ?
Mn2 N1 2.312(2) . ?
O1 H1A 0.8896 . ?
O1 H1B 0.8909 . ?
N1 H1C 0.8900 . ?
N1 H1D 0.8900 . ?
N1 N2 1.440(3) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?
N9 H9A 0.8900 . ?
N9 H9B 0.8900 . ?
N9 H9C 0.8900 . ?
N9 N10 1.420(4) . ?
N8 H8A 0.8900 . ?
N8 H8B 0.8900 . ?
N8 H8C 0.8900 . ?
N8 N7 1.438(3) . ?
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
N4 H4C 0.8900 . ?
N4 N3 1.446(4) . ?
N7 H7A 0.8900(10) . ?
N7 H7B 0.8900(10) . ?
N6 H6A 0.8900 . ?
N6 H6B 0.8900 . ?
N6 H6C 0.8900 . ?
N6 N5 1.395(4) . ?
N10 H10A 0.8900(10) . ?
N10 H10B 0.8900(10) . ?
N3 H3A 0.8901(10) . ?
N3 H3B 0.8900(10) . ?
N5 H5A 0.8604 . ?
N5 H5B 0.8605 . ?

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
Cl3 Mn1 Cl3 180.0 . 2_466 ?
Cl3 Mn1 Cl2 89.27(2) . 2_466 ?
Cl3 Mn1 Cl2 90.73(2) . . ?
Cl3 Mn1 Cl2 89.27(2) 2_466 . ?
Cl3 Mn1 Cl2 90.73(2) 2_466 2_466 ?
Cl2 Mn1 Cl2 180.0 . 2_466 ?
Cl1 Mn1 Cl3 89.82(2) 2_466 . ?
Cl1 Mn1 Cl3 89.82(2) . 2_466 ?
Cl1 Mn1 Cl3 90.18(2) 2_466 2_466 ?
Cl1 Mn1 Cl3 90.18(2) . . ?
Cl1 Mn1 Cl2 92.38(2) 2_466 2_466 ?
Cl1 Mn1 Cl2 87.62(2) . 2_466 ?
Cl1 Mn1 Cl2 92.38(2) . . ?
Cl1 Mn1 Cl2 87.62(2) 2_466 . ?
Cl1 Mn1 Cl1 180.0 2_466 . ?
Cl5 Mn2 Cl6 93.09(2) . . ?
Cl7 Mn2 Cl5 95.37(3) . . ?
Cl7 Mn2 Cl4 171.48(3) . . ?
Cl7 Mn2 Cl6 91.06(2) . . ?
Cl4 Mn2 Cl5 92.62(2) . . ?
Cl4 Mn2 Cl6 91.44(2) . . ?
O1 Mn2 Cl5 87.03(5) . . ?
O1 Mn2 Cl7 91.64(5) . . ?
O1 Mn2 Cl4 85.83(5) . . ?
O1 Mn2 Cl6 177.27(5) . . ?
O1 Mn2 N1 86.26(7) . . ?
N1 Mn2 Cl5 169.81(6) . . ?
N1 Mn2 Cl7 92.48(6) . . ?
N1 Mn2 Cl4 79.25(5) . . ?
N1 Mn2 Cl6 93.25(5) . . ?
Mn2 O1 H1A 111.3 . . ?
Mn2 O1 H1B 111.7 . . ?
H1A O1 H1B 107.2 . . ?
Mn2 N1 H1C 106.9 . . ?
Mn2 N1 H1D 106.9 . . ?
H1C N1 H1D 106.7 . . ?
N2 N1 Mn2 121.62(15) . . ?
N2 N1 H1C 106.9 . . ?
N2 N1 H1D 106.9 . . ?
N1 N2 H2A 109.5 . . ?
N1 N2 H2B 109.5 . . ?
N1 N2 H2C 109.5 . . ?
H2A N2 H2B 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
H9A N9 H9B 109.5 . . ?
H9A N9 H9C 109.5 . . ?
H9B N9 H9C 109.5 . . ?
N10 N9 H9A 109.5 . . ?
N10 N9 H9B 109.5 . . ?
N10 N9 H9C 109.5 . . ?
H8A N8 H8B 109.5 . . ?
H8A N8 H8C 109.5 . . ?
H8B N8 H8C 109.5 . . ?
N7 N8 H8A 109.5 . . ?
N7 N8 H8B 109.5 . . ?
N7 N8 H8C 109.5 . . ?
H4A N4 H4B 109.5 . . ?
H4A N4 H4C 109.5 . . ?
H4B N4 H4C 109.5 . . ?
N3 N4 H4A 109.5 . . ?
N3 N4 H4B 109.5 . . ?
N3 N4 H4C 109.5 . . ?
N8 N7 H7A 109(2) . . ?
N8 N7 H7B 104(2) . . ?
H7A N7 H7B 106.7(3) . . ?
H6A N6 H6B 109.5 . . ?
H6A N6 H6C 109.5 . . ?
H6B N6 H6C 109.5 . . ?
N5 N6 H6A 109.5 . . ?
N5 N6 H6B 109.5 . . ?
N5 N6 H6C 109.5 . . ?
N9 N10 H10A 108(2) . . ?
N9 N10 H10B 104(2) . . ?
H10A N10 H10B 106.7(3) . . ?
N4 N3 H3A 101(3) . . ?
N4 N3 H3B 109(3) . . ?
H3A N3 H3B 106.6(3) . . ?
N6 N5 H5A 108.4 . . ?
N6 N5 H5B 109.6 . . ?
H5A N5 H5B 109.5 . . ?

_iucr_refine_instructions_details 
;

    18_pjs041.res created by SHELXL-2014/7

TITL 18_pjs041_a.res in P-1
REM Old TITL 18_PJS041 in P-1 #2
REM SHELXT solution in P-1
REM R1 0.082, Rweak 0.008, Alpha 0.032, Orientation as input
REM Formula found by SHELXT: N5 O2 Cl16 Mn3
CELL 1.54184 7.583909 9.175246 15.065625 89.8211 84.4469 75.6967
ZERR 1 0.000277 0.000401 0.00063 0.0035 0.0032 0.0035
LATT 1
SFAC Cl H Mn N O
UNIT 16 54 3 20 2
DFIX 0.89 0.001 N3 H3a N3 H3b N7 H7a N7 H7b N10 H10a N10 H10b
DANG 1.428 0.002 H3a H3b H7a H7b H10a H10b
 
L.S. 30
PLAN  13
BOND $H
LIST 6
MORE -1
CONF
fmap 2
acta 136
REM <olex2.extras>
REM <HklSrc "%./18_PJS041.hkl">
REM </olex2.extras>
 
WGHT    0.037700    0.499500
FVAR       4.70835
MN1   3   -0.500000    0.500000    0.500000    10.50000    0.01806    0.01742 =
         0.01321    0.00107    0.00048   -0.00377
MN2   3    0.951299    0.053115    0.188772    11.00000    0.01867    0.01651 =
         0.01465   -0.00010    0.00012   -0.00573
CL3   1   -0.249383    0.558431    0.389262    11.00000    0.02072    0.02856 =
         0.02003    0.00328    0.00330   -0.00742
CL2   1   -0.298863    0.494565    0.629363    11.00000    0.02569    0.02423 =
         0.02078   -0.00154   -0.00705   -0.00496
CL1   1   -0.645742    0.780896    0.523721    11.00000    0.03079    0.01898 =
         0.01948    0.00114    0.00175   -0.00313
CL5   1    1.240239   -0.094643    0.102032    11.00000    0.02341    0.02944 =
         0.02069   -0.00401    0.00482   -0.00556
CL7   1    0.751479   -0.098649    0.134672    11.00000    0.03034    0.02760 =
         0.02241   -0.00198   -0.00468   -0.01398
CL4   1    1.110150    0.236351    0.249048    11.00000    0.02380    0.02343 =
         0.02161   -0.00236   -0.00196   -0.01168
CL6   1    1.003579   -0.108410    0.324125    11.00000    0.03484    0.02212 =
         0.01665    0.00430   -0.00298   -0.00739
CL8   1    0.649497    0.519421    0.126421    11.00000    0.04995    0.02786 =
         0.04036    0.00895   -0.01146   -0.01000
O1    5    0.911098    0.206454    0.069455    11.00000    0.03857    0.02670 =
         0.01884    0.00153   -0.00782   -0.00658
AFIX   7
H1A   2    0.827033    0.291717    0.083433    11.00000   -1.50000
H1B   2    0.874367    0.163054    0.024226    11.00000   -1.50000
AFIX   0
N1    4    0.705432    0.225717    0.261657    11.00000    0.02049    0.02154 =
         0.01606   -0.00106   -0.00090   -0.00745
AFIX  23
H1C   2    0.725830    0.227299    0.318795    11.00000   -1.20000
H1D   2    0.708926    0.315707    0.240446    11.00000   -1.20000
AFIX   0
N2    4    0.520718    0.212150    0.259554    11.00000    0.02001    0.02680 =
         0.02711   -0.00568    0.00053   -0.00368
AFIX 137
H2A   2    0.492374    0.217434    0.203475    11.00000   -1.20000
H2B   2    0.444407    0.286480    0.292061    11.00000   -1.20000
H2C   2    0.511212    0.124150    0.281827    11.00000   -1.20000
AFIX   0
 
N9    4   -0.053789    0.721979    0.526235    11.00000    0.02700    0.02567 =
         0.02956    0.00288   -0.00371   -0.00632
AFIX 137
H9A   2   -0.087070    0.673756    0.482051    11.00000   -1.20000
H9B   2   -0.063418    0.672496    0.576660    11.00000   -1.20000
H9C   2    0.061552    0.727131    0.513499    11.00000   -1.20000
AFIX   0
 
N8    4    0.004952    0.586607    0.217786    11.00000    0.03111    0.02465 =
         0.02179   -0.00049   -0.00145   -0.00504
AFIX 137
H8A   2   -0.096588    0.603337    0.190223    11.00000   -1.20000
H8B   2   -0.000329    0.664186    0.254125    11.00000   -1.20000
H8C   2    0.015314    0.503247    0.249318    11.00000   -1.20000
AFIX   0
 
N4    4    0.455911   -0.190228    0.293351    11.00000    0.03362    0.03919 =
         0.04053    0.01569   -0.00533   -0.01193
AFIX 137
H4A   2    0.494618   -0.192519    0.235566    11.00000   -1.20000
H4B   2    0.334300   -0.169005    0.300073    11.00000   -1.20000
H4C   2    0.500959   -0.279482    0.316507    11.00000   -1.20000
AFIX   0
 
N7    4    0.160792    0.568920    0.152664    11.00000    0.05020    0.02926 =
         0.03814   -0.00213    0.01730   -0.01562
H7A   2    0.261215    0.552770    0.181076    11.00000   -1.20000
H7B   2    0.147128    0.659197    0.128523    11.00000   -1.20000
N6    4    0.274458    0.282066    0.041833    11.00000    0.04883    0.04896 =
         0.02076   -0.00363   -0.00656   -0.01324
AFIX 137
H6A   2    0.293347    0.312787   -0.013573    11.00000   -1.20000
H6B   2    0.222511    0.361269    0.077503    11.00000   -1.20000
H6C   2    0.201131    0.219742    0.042694    11.00000   -1.20000
AFIX   0
 
N10   4   -0.169331    0.869625    0.536593    11.00000    0.05960    0.03738 =
         0.03006    0.00223    0.00262    0.01026
H10A  2   -0.154081    0.918170    0.486310    11.00000   -1.20000
H10B  2   -0.122336    0.912633    0.578307    11.00000   -1.20000
N3    4    0.517438   -0.075938    0.338708    11.00000    0.05474    0.04624 =
         0.02925    0.00508    0.00543   -0.01587
H3A   2    0.633783   -0.122636    0.343415    11.00000   -1.20000
H3B   2    0.461808   -0.062788    0.393927    11.00000   -1.20000
N5    4    0.441249    0.207437    0.071428    11.00000    0.02928    0.10005 =
         0.02784   -0.00966    0.00286    0.00373
AFIX   7
H5A   2    0.428400    0.125576    0.096199    11.00000   -1.20000
H5B   2    0.523633    0.186256    0.026764    11.00000   -1.20000
AFIX   0
HKLF 4
 
REM  18_pjs041_a.res in P-1
REM R1 =  0.0316 for    3644 Fo > 4sig(Fo)  and  0.0341 for all    3911 data
REM    212 parameters refined using      9 restraints
 
END  
     
WGHT      0.0377      0.4999 

REM Highest difference peak  0.535,  deepest hole -0.534,  1-sigma level  0.088
Q1    1   0.3984 -0.0635  0.3256  11.00000  0.05    0.53
Q2    1   0.4972  0.2786  0.0635  11.00000  0.05    0.35
Q3    1   0.9300  0.1109  0.2593  11.00000  0.05    0.35
Q4    1   1.0037  0.2199  0.2750  11.00000  0.05    0.34
Q5    1   0.7557  0.5057  0.0957  11.00000  0.05    0.33
Q6    1  -0.2670  0.4814  0.4839  11.00000  0.05    0.33
Q7    1   0.2873  0.2160 -0.0181  11.00000  0.05    0.30
Q8    1   1.2022  0.0214  0.1863  11.00000  0.05    0.30
Q9    1  -0.5880  0.7229  0.4417  11.00000  0.05    0.29
Q10   1   0.8801 -0.1024  0.1037  11.00000  0.05    0.29
Q11   1   0.7037  0.0615  0.1881  11.00000  0.05    0.28
Q12   1   0.4212  0.0636  0.0691  11.00000  0.05    0.28
Q13   1   1.0001  0.3016  0.1970  11.00000  0.05    0.27

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0316 for 3644 Fo > 4sig(Fo) and 0.0341 for all 6591 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.53, deepest hole -0.53
  REM Mean Shift 0, Max Shift 0.001.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0341
  REM R1_gt = 0.0316
  REM wR_ref = 0.0818
  REM GOOF = 1.050
  REM Shift_max = 0.001
  REM Shift_mean = 0
  REM Reflections_all = 6591
  REM Reflections_gt = 3644
  REM Parameters = n/a
  REM Hole = -0.53
  REM Peak = 0.53
  REM Flack = n/a

  
;
_olex2_date_sample_data_collection 2018-01-18
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.921
_oxdiff_exptl_absorpt_empirical_full_min 0.682
####################################################################### 
# 
# 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_18_pjs_044_Hyd3MnCl5
_database_code_depnum_ccdc_archive 'CCDC 1877364'
_audit_update_record             
;
2018-11-06 deposited with the CCDC.
2018-12-27 downloaded from the CCDC.
;
_audit_creation_date             2018-02-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3461 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cl5 H5 Mn N2, 2(H5 N2)'
_chemical_formula_sum            'Cl5 H15 Mn N6'
_chemical_formula_weight         331.37
_chemical_melting_point          ?
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'
N N 0.0061 0.0033 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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                   8.9779(4)
_cell_length_b                   10.9705(4)
_cell_length_c                   11.7726(5)
_cell_angle_alpha                90
_cell_angle_beta                 94.423(4)
_cell_angle_gamma                90
_cell_volume                     1156.05(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4466
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.2820
_cell_measurement_theta_min      4.3520
_shelx_estimated_absorpt_T_max   0.886
_shelx_estimated_absorpt_T_min   0.606
_exptl_absorpt_coefficient_mu    2.262
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64560
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.904
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             668
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.246
_exptl_crystal_size_mid          0.221
_exptl_crystal_size_min          0.055
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0237
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.869
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10289
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.869
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.786
_diffrn_reflns_theta_min         3.321
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2887
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.869
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -14.00  29.00   1.00   10.00    --   11.79  57.00 -60.00   43
  2  ω     50.00  76.00   1.00   10.00    --   11.79  57.00 -60.00   26
  3  ω     50.00  83.00   1.00   10.00    --   11.79  57.00 -90.00   33
  4  ω     14.00  86.00   1.00   10.00    --   11.79  38.00-150.00   72
  5  ω      1.00  30.00   1.00   10.00    --  -10.46 -99.00-150.00   29
  6  ω    -20.00  46.00   1.00   10.00    --   11.79 -99.00  30.00   66
  7  ω    -20.00  46.00   1.00   10.00    --   11.79 -99.00 120.00   66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0606679000
_diffrn_orient_matrix_UB_12      -0.0357274000
_diffrn_orient_matrix_UB_13      0.0234452000
_diffrn_orient_matrix_UB_21      0.0214167000
_diffrn_orient_matrix_UB_22      0.0479266000
_diffrn_orient_matrix_UB_23      0.0383027000
_diffrn_orient_matrix_UB_31      -0.0462451000
_diffrn_orient_matrix_UB_32      -0.0246059000
_diffrn_orient_matrix_UB_33      0.0404633000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2432
_reflns_number_total             2878
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         2878
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0323
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0309P)²+1.1186P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0801
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups, All N(H,H,H) groups
2.a Rotating group:
 N5(H5A,H5B), N3(H3A,H3B)
2.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B)
2.c Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C), N6(H6A,H6B,H6C), N4(H4A,H4B,H4C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.52168(4) 0.74804(3) 0.71927(3) 0.02123(10) Uani 1 1 d . . . . .
Cl2 Cl 0.55558(7) 0.72245(6) 0.93333(5) 0.02964(14) Uani 1 1 d . . . . .
Cl1 Cl 0.23903(6) 0.74639(5) 0.72597(5) 0.02907(14) Uani 1 1 d . . . . .
Cl5 Cl 0.52942(7) 0.51361(5) 0.70577(5) 0.02917(14) Uani 1 1 d . . . . .
Cl3 Cl 0.54023(7) 0.97664(5) 0.75157(5) 0.03162(15) Uani 1 1 d . . . . .
Cl4 Cl 0.50282(8) 0.76879(6) 0.50857(5) 0.03863(16) Uani 1 1 d . . . . .
N2 N 0.8752(2) 0.75172(16) 0.64194(16) 0.0244(4) Uani 1 1 d . . . . .
H2A H 0.8551 0.6890 0.5953 0.029 Uiso 1 1 calc GR . . . .
H2B H 0.9716 0.7508 0.6660 0.029 Uiso 1 1 calc GR . . . .
H2C H 0.8538 0.8211 0.6050 0.029 Uiso 1 1 calc GR . . . .
N1 N 0.7860(2) 0.74237(16) 0.73847(16) 0.0232(4) Uani 1 1 d . . . . .
H1A H 0.8155 0.8022 0.7861 0.028 Uiso 1 1 calc R . . . .
H1B H 0.8116 0.6728 0.7736 0.028 Uiso 1 1 calc R . . . .
N5 N 0.7921(3) 0.5680(2) 0.46595(18) 0.0384(5) Uani 1 1 d . . . . .
H5A H 0.8566 0.5589 0.4162 0.046 Uiso 1 1 d GR . . . .
H5B H 0.7206 0.6139 0.4381 0.046 Uiso 1 1 d GR . . . .
N6 N 0.7347(3) 0.4535(2) 0.4933(2) 0.0411(5) Uani 1 1 d . . . . .
H6A H 0.6876 0.4207 0.4314 0.049 Uiso 1 1 calc GR . . . .
H6B H 0.6708 0.4623 0.5469 0.049 Uiso 1 1 calc GR . . . .
H6C H 0.8092 0.4049 0.5190 0.049 Uiso 1 1 calc GR . . . .
N3 N 0.7655(3) 0.9706(2) 0.5247(2) 0.0431(6) Uani 1 1 d . . . . .
H3A H 0.8110 1.0320 0.5578 0.052 Uiso 1 1 d GR . . . .
H3B H 0.6741 0.9690 0.5429 0.052 Uiso 1 1 d GR . . . .
N4 N 0.7669(3) 0.9819(2) 0.4061(2) 0.0496(6) Uani 1 1 d . . . . .
H4A H 0.7016 0.9299 0.3723 0.060 Uiso 1 1 calc GR . . . .
H4B H 0.8579 0.9654 0.3854 0.060 Uiso 1 1 calc GR . . . .
H4C H 0.7419 1.0577 0.3855 0.060 Uiso 1 1 calc GR . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mn1 0.01971(19) 0.02249(18) 0.02147(18) -0.00123(13) 0.00137(13) -0.00026(12)
Cl2 0.0310(3) 0.0382(3) 0.0199(3) -0.0006(2) 0.0034(2) 0.0043(2)
Cl1 0.0192(3) 0.0350(3) 0.0327(3) -0.0004(2) -0.0002(2) 0.0005(2)
Cl5 0.0299(3) 0.0217(3) 0.0353(3) -0.0010(2) -0.0013(2) 0.0009(2)
Cl3 0.0298(3) 0.0206(3) 0.0442(4) -0.0031(2) 0.0012(2) -0.0014(2)
Cl4 0.0438(4) 0.0483(4) 0.0233(3) 0.0010(3) -0.0006(3) -0.0089(3)
N2 0.0229(10) 0.0262(10) 0.0248(10) -0.0004(7) 0.0058(8) -0.0015(7)
N1 0.0231(10) 0.0267(9) 0.0202(9) -0.0003(7) 0.0036(7) 0.0009(7)
N5 0.0461(14) 0.0333(12) 0.0354(12) 0.0050(9) -0.0007(10) -0.0093(10)
N6 0.0498(15) 0.0347(12) 0.0374(12) -0.0001(10) -0.0062(10) -0.0084(11)
N3 0.0483(15) 0.0343(12) 0.0486(14) 0.0013(10) 0.0164(11) -0.0018(11)
N4 0.0585(17) 0.0502(15) 0.0378(13) -0.0010(11) -0.0107(11) 0.0116(13)

_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 Cl2 2.5306(6) . ?
Mn1 Cl1 2.5450(7) . ?
Mn1 Cl5 2.5780(6) . ?
Mn1 Cl3 2.5400(6) . ?
Mn1 Cl4 2.4837(7) . ?
Mn1 N1 2.368(2) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?
N2 N1 1.443(3) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N5 H5A 0.8609 . ?
N5 H5B 0.8604 . ?
N5 N6 1.405(3) . ?
N6 H6A 0.8900 . ?
N6 H6B 0.8900 . ?
N6 H6C 0.8900 . ?
N3 H3A 0.8647 . ?
N3 H3B 0.8647 . ?
N3 N4 1.402(3) . ?
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
N4 H4C 0.8900 . ?

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
Cl2 Mn1 Cl1 90.69(2) . . ?
Cl2 Mn1 Cl5 87.08(2) . . ?
Cl2 Mn1 Cl3 87.65(2) . . ?
Cl1 Mn1 Cl5 91.52(2) . . ?
Cl3 Mn1 Cl1 93.23(2) . . ?
Cl3 Mn1 Cl5 172.94(2) . . ?
Cl4 Mn1 Cl2 176.80(3) . . ?
Cl4 Mn1 Cl1 92.31(2) . . ?
Cl4 Mn1 Cl5 91.72(2) . . ?
Cl4 Mn1 Cl3 93.30(2) . . ?
N1 Mn1 Cl2 81.91(5) . . ?
N1 Mn1 Cl1 172.52(5) . . ?
N1 Mn1 Cl5 87.03(5) . . ?
N1 Mn1 Cl3 87.59(5) . . ?
N1 Mn1 Cl4 95.07(5) . . ?
H2A N2 H2B 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
N1 N2 H2A 109.5 . . ?
N1 N2 H2B 109.5 . . ?
N1 N2 H2C 109.5 . . ?
Mn1 N1 H1A 106.7 . . ?
Mn1 N1 H1B 106.7 . . ?
N2 N1 Mn1 122.39(14) . . ?
N2 N1 H1A 106.7 . . ?
N2 N1 H1B 106.7 . . ?
H1A N1 H1B 106.6 . . ?
H5A N5 H5B 109.3 . . ?
N6 N5 H5A 109.3 . . ?
N6 N5 H5B 109.5 . . ?
N5 N6 H6A 109.5 . . ?
N5 N6 H6B 109.5 . . ?
N5 N6 H6C 109.5 . . ?
H6A N6 H6B 109.5 . . ?
H6A N6 H6C 109.5 . . ?
H6B N6 H6C 109.5 . . ?
H3A N3 H3B 109.1 . . ?
N4 N3 H3A 109.8 . . ?
N4 N3 H3B 109.3 . . ?
N3 N4 H4A 109.5 . . ?
N3 N4 H4B 109.5 . . ?
N3 N4 H4C 109.5 . . ?
H4A N4 H4B 109.5 . . ?
H4A N4 H4C 109.5 . . ?
H4B N4 H4C 109.5 . . ?

_iucr_refine_instructions_details 
;

    18_pjs_044.res created by SHELXL-2014/7

TITL 18_pjs_044_a.res in P2(1)/n
REM Old TITL 18_PJS_044 in P21/n #14
REM SHELXT solution in P2(1)/n
REM R1 0.090, Rweak 0.002, Alpha 0.018, Orientation as input
REM Formula found by SHELXT: Mn Cl5 N6
CELL 0.71073 8.97788 10.970509 11.772593 90 94.4225 90
ZERR 4 0.000413 0.000441 0.000485 0 0.0038 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC Mn Cl N H
UNIT 4 20 24 60
 
L.S. 4
PLAN  20
SIZE 0.246 0.221 0.055
BOND $H
LIST 6
MORE -1
CONF
fmap 2
acta 52
REM <olex2.extras>
REM <HklSrc "%./18_PJS_044.hkl">
REM </olex2.extras>
 
WGHT    0.030900    1.118600
FVAR       0.31580
MN1   1    0.521681    0.748037    0.719274    11.00000    0.01971    0.02249 =
         0.02147   -0.00123    0.00137   -0.00026
CL2   2    0.555583    0.722450    0.933334    11.00000    0.03102    0.03823 =
         0.01989   -0.00056    0.00344    0.00427
CL1   2    0.239027    0.746387    0.725972    11.00000    0.01925    0.03497 =
         0.03266   -0.00036   -0.00019    0.00052
CL5   2    0.529415    0.513606    0.705765    11.00000    0.02992    0.02168 =
         0.03531   -0.00096   -0.00134    0.00092
CL3   2    0.540226    0.976637    0.751565    11.00000    0.02982    0.02062 =
         0.04416   -0.00310    0.00120   -0.00138
CL4   2    0.502818    0.768791    0.508574    11.00000    0.04385    0.04827 =
         0.02327    0.00095   -0.00063   -0.00895
N2    3    0.875199    0.751715    0.641937    11.00000    0.02294    0.02615 =
         0.02479   -0.00035    0.00579   -0.00154
AFIX 137
H2A   4    0.855147    0.689034    0.595250    11.00000   -1.20000
H2B   4    0.971630    0.750790    0.666013    11.00000   -1.20000
H2C   4    0.853798    0.821086    0.605020    11.00000   -1.20000
AFIX   0
N1    3    0.786049    0.742367    0.738469    11.00000    0.02309    0.02672 =
         0.02019   -0.00029    0.00363    0.00088
AFIX  23
H1A   4    0.815519    0.802169    0.786111    11.00000   -1.20000
H1B   4    0.811643    0.672772    0.773599    11.00000   -1.20000
AFIX   0
 
N5    3    0.792061    0.568004    0.465949    11.00000    0.04605    0.03329 =
         0.03538    0.00496   -0.00074   -0.00934
AFIX   7
H5A   4    0.856569    0.558885    0.416177    11.00000   -1.20000
H5B   4    0.720561    0.613875    0.438110    11.00000   -1.20000
AFIX   0
N6    3    0.734661    0.453486    0.493330    11.00000    0.04979    0.03469 =
         0.03742   -0.00007   -0.00616   -0.00838
AFIX 137
H6A   4    0.687603    0.420656    0.431410    11.00000   -1.20000
H6B   4    0.670770    0.462302    0.546913    11.00000   -1.20000
H6C   4    0.809243    0.404948    0.519015    11.00000   -1.20000
AFIX   0
 
N3    3    0.765515    0.970601    0.524663    11.00000    0.04829    0.03429 =
         0.04857    0.00133    0.01639   -0.00184
AFIX   7
H3A   4    0.810973    1.032012    0.557763    11.00000   -1.20000
H3B   4    0.674075    0.969040    0.542943    11.00000   -1.20000
AFIX   0
N4    3    0.766853    0.981939    0.406143    11.00000    0.05854    0.05019 =
         0.03782   -0.00096   -0.01072    0.01164
AFIX 137
H4A   4    0.701592    0.929914    0.372260    11.00000   -1.20000
H4B   4    0.857945    0.965380    0.385419    11.00000   -1.20000
H4C   4    0.741874    1.057720    0.385502    11.00000   -1.20000
AFIX   0
HKLF 4
 
REM  18_pjs_044_a.res in P2(1)/n
REM R1 =  0.0323 for    2432 Fo > 4sig(Fo)  and  0.0403 for all    2878 data
REM    114 parameters refined using      0 restraints
 
END  
     
WGHT      0.0309      1.1186 

REM Highest difference peak  0.651,  deepest hole -0.539,  1-sigma level  0.092
Q1    1   0.8145  0.4684  0.4399  11.00000  0.05    0.65
Q2    1   0.7194  0.5693  0.5062  11.00000  0.05    0.47
Q3    1   0.7165  0.9245  0.4837  11.00000  0.05    0.39
Q4    1   0.6869  1.0231  0.4800  11.00000  0.05    0.38
Q5    1   0.8146  0.9260  0.4665  11.00000  0.05    0.37
Q6    1   0.4529  0.7198  0.5108  11.00000  0.05    0.33
Q7    1   0.5971  0.7811  0.9419  11.00000  0.05    0.30
Q8    1   0.6502  0.8260  0.6201  11.00000  0.05    0.29
Q9    1   1.0903  0.8566  0.6831  11.00000  0.05    0.27
Q10   1   0.5926  0.5815  0.6722  11.00000  0.05    0.25
Q11   1   0.6940  0.8852  0.5791  11.00000  0.05    0.25
Q12   1   0.6348  1.1158  0.4324  11.00000  0.05    0.25
Q13   1   0.4747  0.6390  0.8957  11.00000  0.05    0.25
Q14   1   0.5681  0.7320  0.5269  11.00000  0.05    0.25
Q15   1   0.6108  0.8258  0.4700  11.00000  0.05    0.25
Q16   1   1.0900  0.6027  0.6594  11.00000  0.05    0.24
Q17   1   0.7913  0.6075  0.6817  11.00000  0.05    0.24
Q18   1   0.3939  0.6516  0.7603  11.00000  0.05    0.24
Q19   1   0.8664  0.9053  0.5394  11.00000  0.05    0.23
Q20   1   0.6658  0.8575  0.5493  11.00000  0.05    0.23

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0323 for 2432 Fo > 4sig(Fo) and 0.0403 for all 10580 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.65, deepest hole -0.54
  REM Mean Shift 0, Max Shift 0.001.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0403
  REM R1_gt = 0.0323
  REM wR_ref = 0.0801
  REM GOOF = 1.044
  REM Shift_max = 0.001
  REM Shift_mean = 0
  REM Reflections_all = 10580
  REM Reflections_gt = 2432
  REM Parameters = n/a
  REM Hole = -0.54
  REM Peak = 0.65
  REM Flack = n/a

  
;
_olex2_date_sample_data_collection 2018-01-25
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.221
_oxdiff_exptl_absorpt_empirical_full_min 0.775
####################################################################### 
# 
# 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_18_pjs042_HydMnCl3
_database_code_depnum_ccdc_archive 'CCDC 1877365'
_audit_update_record             
;
2018-11-06 deposited with the CCDC.
2018-12-27 downloaded from the CCDC.
;
_audit_creation_date             2018-02-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3461 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cl3 H9 Mn N2 O2'
_chemical_formula_sum            'Cl3 H9 Mn N2 O2'
_chemical_formula_weight         230.38
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 '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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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                   5.54110(10)
_cell_length_b                   13.9707(3)
_cell_length_c                   9.9630(3)
_cell_angle_alpha                90
_cell_angle_beta                 92.648(2)
_cell_angle_gamma                90
_cell_volume                     770.44(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1718
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.6710
_cell_measurement_theta_min      5.4740
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    22.989
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74412
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.986
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.057
_exptl_crystal_size_min          0.038
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2816
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         72.820
_diffrn_reflns_theta_min         5.457
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2887
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -55.00 -29.00   1.00    1.00    --  -41.91 -57.00   0.00   26
  2  ω   -114.00 -17.00   1.00    1.00    --  -41.91 -38.00-120.00   97
  3  ω   -114.00 -88.00   1.00    1.00    --  -41.91 -57.00   0.00   26
  4  ω      7.00  46.00   1.00    1.00    --   41.91 -99.00 120.00   39
  5  ω     53.00  83.00   1.00    1.00    --   41.91 -99.00 120.00   30
  6  ω     49.00 121.00   1.00    3.41    --  105.91-125.00 -30.00   72
  7  ω     36.00  94.00   1.00    3.41    --  105.91 -61.00 -30.00   58
  8  ω     84.00 177.00   1.00    3.41    --  105.91  30.00  90.00   93
  9  ω    153.00 178.00   1.00    3.41    --  105.91 128.00 175.00   25
 10  ω    102.00 155.00   1.00    3.41    --  105.91 125.00  90.00   53
 11  ω    110.00 164.00   1.00    3.41    --  105.91 125.00 -30.00   54
 12  ω     88.00 123.00   1.00    3.41    --  105.91  45.00-120.00   35
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0851158000
_diffrn_orient_matrix_UB_12      -0.0834542000
_diffrn_orient_matrix_UB_13      0.0914266000
_diffrn_orient_matrix_UB_21      0.0795274000
_diffrn_orient_matrix_UB_22      0.0717978000
_diffrn_orient_matrix_UB_23      0.1107771000
_diffrn_orient_matrix_UB_31      -0.2529322000
_diffrn_orient_matrix_UB_32      -0.0055776000
_diffrn_orient_matrix_UB_33      0.0576554000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1376
_reflns_number_total             1486
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.332
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     76
_refine_ls_number_reflns         1486
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0270
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0332P)²+0.0115P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0660
_refine_ls_wR_factor_ref         0.0688
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O2(H2A,H2B), O1(H1A,H1B)
2.b Secondary CH2 refined with riding coordinates:
 N1(H1C,H1D)
2.c Idealised Me refined as rotating group:
 N2(H2C,H2D,H2E)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.51640(6) 0.34928(3) 0.23927(3) 0.01954(13) Uani 1 1 d . . . . .
Cl3 Cl 0.24235(10) 0.44547(5) 0.09075(6) 0.02797(15) Uani 1 1 d . . . . .
Cl2 Cl 0.29008(11) 0.38952(4) 0.44264(5) 0.02846(16) Uani 1 1 d . . . . .
Cl1 Cl 0.32275(11) 0.18943(4) 0.20107(6) 0.02977(16) Uani 1 1 d . . . . .
O2 O 0.7961(3) 0.27987(14) 0.37678(19) 0.0326(4) Uani 1 1 d . . . . .
H2A H 0.7730 0.2949 0.4599 0.049 Uiso 1 1 d GR . . . .
H2B H 0.9387 0.3029 0.3632 0.049 Uiso 1 1 d GR . . . .
O1 O 0.7619(4) 0.31819(15) 0.0792(2) 0.0393(5) Uani 1 1 d . . . . .
H1A H 0.7923 0.2582 0.0774 0.059 Uiso 1 1 d GR . . . .
H1B H 0.8993 0.3440 0.0982 0.059 Uiso 1 1 d GR . . . .
N1 N 0.7582(4) 0.48712(15) 0.2788(2) 0.0272(4) Uani 1 1 d . . . . .
H1C H 0.7778 0.4948 0.3673 0.033 Uiso 1 1 calc R . . . .
H1D H 0.9034 0.4752 0.2479 0.033 Uiso 1 1 calc R . . . .
N2 N 0.6757(5) 0.57657(16) 0.2225(2) 0.0338(5) Uani 1 1 d . . . . .
H2C H 0.6624 0.5718 0.1334 0.041 Uiso 1 1 calc GR . . . .
H2D H 0.7811 0.6225 0.2455 0.041 Uiso 1 1 calc GR . . . .
H2E H 0.5323 0.5910 0.2539 0.041 Uiso 1 1 calc GR . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mn1 0.0221(2) 0.0166(2) 0.01986(19) 0.00000(13) 0.00025(14) -0.00046(13)
Cl3 0.0263(3) 0.0309(3) 0.0263(3) 0.0074(2) -0.0028(2) 0.0020(2)
Cl2 0.0343(3) 0.0291(3) 0.0224(3) -0.0044(2) 0.0059(2) -0.0022(2)
Cl1 0.0327(3) 0.0202(3) 0.0362(3) -0.0009(2) -0.0013(2) -0.0065(2)
O2 0.0282(9) 0.0358(10) 0.0331(9) 0.0047(8) -0.0065(7) -0.0010(8)
O1 0.0386(11) 0.0317(11) 0.0491(12) -0.0143(9) 0.0173(9) -0.0099(8)
N1 0.0306(11) 0.0215(10) 0.0295(10) -0.0043(9) 0.0008(8) -0.0003(8)
N2 0.0480(13) 0.0216(11) 0.0317(11) -0.0012(9) -0.0014(10) -0.0062(10)

_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 Cl3 2.4686(7) . ?
Mn1 Cl2 2.4958(6) . ?
Mn1 Cl1 2.4991(7) . ?
Mn1 O2 2.2413(18) . ?
Mn1 O1 2.1873(18) . ?
Mn1 N1 2.369(2) . ?
O2 H2A 0.8694 . ?
O2 H2B 0.8695 . ?
O1 H1A 0.8558 . ?
O1 H1B 0.8555 . ?
N1 H1C 0.8900 . ?
N1 H1D 0.8900 . ?
N1 N2 1.436(3) . ?
N2 H2C 0.8900 . ?
N2 H2D 0.8900 . ?
N2 H2E 0.8900 . ?

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
Cl3 Mn1 Cl2 92.62(2) . . ?
Cl3 Mn1 Cl1 98.47(2) . . ?
Cl2 Mn1 Cl1 95.54(2) . . ?
O2 Mn1 Cl3 172.23(6) . . ?
O2 Mn1 Cl2 87.73(5) . . ?
O2 Mn1 Cl1 89.22(5) . . ?
O2 Mn1 N1 83.13(7) . . ?
O1 Mn1 Cl3 93.27(7) . . ?
O1 Mn1 Cl2 171.71(6) . . ?
O1 Mn1 Cl1 89.35(6) . . ?
O1 Mn1 O2 85.64(8) . . ?
O1 Mn1 N1 85.21(7) . . ?
N1 Mn1 Cl3 89.11(6) . . ?
N1 Mn1 Cl2 89.06(5) . . ?
N1 Mn1 Cl1 170.91(6) . . ?
Mn1 O2 H2A 110.5 . . ?
Mn1 O2 H2B 110.6 . . ?
H2A O2 H2B 103.5 . . ?
Mn1 O1 H1A 109.8 . . ?
Mn1 O1 H1B 109.4 . . ?
H1A O1 H1B 104.1 . . ?
Mn1 N1 H1C 107.7 . . ?
Mn1 N1 H1D 107.7 . . ?
H1C N1 H1D 107.1 . . ?
N2 N1 Mn1 118.38(15) . . ?
N2 N1 H1C 107.7 . . ?
N2 N1 H1D 107.7 . . ?
N1 N2 H2C 109.5 . . ?
N1 N2 H2D 109.5 . . ?
N1 N2 H2E 109.5 . . ?
H2C N2 H2D 109.5 . . ?
H2C N2 H2E 109.5 . . ?
H2D N2 H2E 109.5 . . ?

_iucr_refine_instructions_details 
;

    18_pjs042.res created by SHELXL-2014/7

TITL 18_pjs042_a.res in P2(1)/n
REM Old TITL 18_PJS042 in P21/n #14
REM SHELXT solution in P2(1)/n
REM R1 0.296, Rweak 0.015, Alpha 0.018, Orientation as input
REM Formula found by SHELXT: C2 N O
CELL 1.54184 5.5411 13.9707 9.963 90 92.648 90
ZERR 4 0.0001 0.0003 0.0003 0 0.002 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC Mn Cl N H O
UNIT 4 12 8 36 8
 
L.S. 20
PLAN  20
BOND $H
list 4
fmap 2
acta 134
REM <olex2.extras>
REM <HklSrc "%./18_PJS042.hkl">
REM </olex2.extras>
 
WGHT    0.033200    0.011500
FVAR       0.65539
MN1   1    0.516397    0.349280    0.239270    11.00000    0.02206    0.01664 =
         0.01986    0.00000    0.00025   -0.00046
CL3   2    0.242346    0.445474    0.090753    11.00000    0.02627    0.03093 =
         0.02634    0.00744   -0.00282    0.00202
CL2   2    0.290082    0.389520    0.442640    11.00000    0.03431    0.02908 =
         0.02242   -0.00439    0.00587   -0.00222
CL1   2    0.322749    0.189433    0.201067    11.00000    0.03269    0.02016 =
         0.03620   -0.00086   -0.00131   -0.00652
O2    5    0.796113    0.279866    0.376777    11.00000    0.02818    0.03579 =
         0.03310    0.00470   -0.00650   -0.00097
AFIX   7
H2A   4    0.772974    0.294887    0.459887    11.00000   -1.50000
H2B   4    0.938693    0.302936    0.363236    11.00000   -1.50000
AFIX   0
O1    5    0.761927    0.318195    0.079171    11.00000    0.03855    0.03173 =
         0.04915   -0.01434    0.01726   -0.00993
AFIX   7
H1A   4    0.792251    0.258155    0.077402    11.00000   -1.50000
H1B   4    0.899306    0.343997    0.098179    11.00000   -1.50000
AFIX   0
N1    3    0.758207    0.487125    0.278760    11.00000    0.03059    0.02150 =
         0.02951   -0.00426    0.00082   -0.00027
AFIX  23
H1C   4    0.777807    0.494764    0.367278    11.00000   -1.20000
H1D   4    0.903373    0.475241    0.247881    11.00000   -1.20000
AFIX   0
N2    3    0.675663    0.576573    0.222546    11.00000    0.04797    0.02160 =
         0.03165   -0.00125   -0.00138   -0.00622
AFIX 137
H2C   4    0.662449    0.571752    0.133436    11.00000   -1.20000
H2D   4    0.781095    0.622458    0.245476    11.00000   -1.20000
H2E   4    0.532270    0.590964    0.253878    11.00000   -1.20000
AFIX   0
HKLF 4
 
REM  18_pjs042_a.res in P2(1)/n
REM R1 =  0.0270 for    1376 Fo > 4sig(Fo)  and  0.0297 for all    1486 data
REM     76 parameters refined using      0 restraints
 
END  
     
WGHT      0.0332      0.0115 

REM Highest difference peak  0.332,  deepest hole -0.343,  1-sigma level  0.094
Q1    1   0.2319  0.5416  0.1361  11.00000  0.05    0.33
Q2    1   0.5000  0.5000  0.0000  10.50000  0.05    0.31
Q3    1   0.8871  0.4388  0.0004  11.00000  0.05    0.30
Q4    1   0.5521  0.4718  0.2237  11.00000  0.05    0.30
Q5    1   0.5042  0.4467  0.2656  11.00000  0.05    0.28
Q6    1   0.2594  0.5403  0.0680  11.00000  0.05    0.27
Q7    1   0.7607  0.1933  0.0184  11.00000  0.05    0.27
Q8    1   0.5433  0.2625  0.1683  11.00000  0.05    0.26
Q9    1   0.6651  0.4261  0.1566  11.00000  0.05    0.26
Q10   1   0.3629  0.3184  0.3590  11.00000  0.05    0.25
Q11   1   0.2157  0.3730  0.0412  11.00000  0.05    0.25
Q12   1   0.2652  0.3594  0.0523  11.00000  0.05    0.25
Q13   1   0.2977  0.4620  0.4432  11.00000  0.05    0.25
Q14   1   0.1609  0.5197 -0.0410  11.00000  0.05    0.24
Q15   1   0.3838  0.0731  0.1651  11.00000  0.05    0.24
Q16   1   0.4948  0.2554  0.2856  11.00000  0.05    0.24
Q17   1   0.7570  0.2552  0.0218  11.00000  0.05    0.24
Q18   1   0.7983  0.3906  0.2740  11.00000  0.05    0.24
Q19   1   0.7525  0.3568  0.2994  11.00000  0.05    0.23
Q20   1   0.1811  0.3535  0.1552  11.00000  0.05    0.23

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0270 for 1376 Fo > 4sig(Fo) and 0.0297 for all 2914 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.33, deepest hole -0.34
  REM Mean Shift 0, Max Shift -0.001.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0297
  REM R1_gt = 0.0270
  REM wR_ref = 0.0688
  REM GOOF = 1.065
  REM Shift_max = -0.001
  REM Shift_mean = 0
  REM Reflections_all = 2914
  REM Reflections_gt = 1376
  REM Parameters = n/a
  REM Hole = -0.34
  REM Peak = 0.33
  REM Flack = n/a

  
;
_olex2_date_sample_data_collection 2018-01-18
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.463
_oxdiff_exptl_absorpt_empirical_full_min 0.854
####################################################################### 
# 
# 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_18_pjs_019_MHA2CuCl2
_database_code_depnum_ccdc_archive 'CCDC 1877367'
_audit_update_record             
;
2018-11-06 deposited with the CCDC.
2018-12-27 downloaded from the CCDC.
;
_audit_creation_date             2018-07-30
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C2 H10 Cl2 Cu N2 O2'
_chemical_formula_sum            'C2 H10 Cl2 Cu N2 O2'
_chemical_formula_weight         228.56
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Cu C O N H'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 '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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   3.7868(6)
_cell_length_b                   5.6827(9)
_cell_length_c                   8.7079(11)
_cell_angle_alpha                99.853(12)
_cell_angle_beta                 98.563(12)
_cell_angle_gamma                91.568(13)
_cell_volume                     182.30(5)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    2099
_cell_measurement_temperature    150.0(4)
_cell_measurement_theta_max      75.8200
_cell_measurement_theta_min      5.1350
_shelx_estimated_absorpt_T_max   0.834
_shelx_estimated_absorpt_T_min   0.280
_exptl_absorpt_coefficient_mu    10.472
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84600
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.082
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             115
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.163
_exptl_crystal_size_mid          0.022
_exptl_crystal_size_min          0.018
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3563
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         76.510
_diffrn_reflns_theta_min         5.219
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.0(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2774
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -115.00 -17.00   1.00    4.00    --  -41.22 -38.00 -60.00   98
  2  ω   -115.00 -17.00   1.00    4.00    --  -41.22 -38.00  30.00   98
  3  ω    -35.00  74.00   1.00    4.00    --   41.22 -77.00-150.00  109
  4  ω     23.00  97.00   1.00    4.00    --   41.22-125.00-150.00   74
  5  ω     86.00 178.00   1.00    8.00    --  112.00  45.00 -90.00   92
  6  ω     29.00 109.00   1.00    8.00    --  112.00 -94.00  60.00   80
  7  ω     39.00 138.00   1.00    8.00    --  112.00 -45.00  30.00   99
  8  ω     36.00 116.00   1.00    8.00    --  112.00-111.00 -60.00   80
  9  ω    100.00 178.00   1.00    8.00    --  112.00 111.00 120.00   78
 10  ω     86.00 178.00   1.00    8.00    --  112.00  45.00-150.00   92
 11  ω    100.00 178.00   1.00    8.00    --  112.00 111.00  90.00   78
 12  ω     29.00 109.00   1.00    8.00    --  112.00 -94.00 -30.00   80
 13  ω     57.00 151.00   1.00    8.00    --  112.00 178.00 -90.00   94
 14  ω     57.00 151.00   1.00    8.00    --  112.00 178.00 -30.00   94
 15  ω     79.00 178.00   1.00    8.00    --  112.00  77.00   0.00   99
 16  ω   -113.00 -65.00   1.00    4.00    --  -41.22-138.00-112.00   48
 17  ω   -113.00 -13.00   1.00    4.00    --  -41.22 -57.00-120.00  100
 18  ω   -113.00 -13.00   1.00    4.00    --  -41.22 -57.00 150.00  100
 19  ω      9.00 117.00   1.00    4.00    --   41.22  77.00  30.00  108
 20  ω      1.00  82.00   1.00    4.00    --   41.22 -99.00 -60.00   81
 21  ω     83.00 178.00   1.00    8.00    --  112.00  61.00 150.00   95
 22  ω     79.00 178.00   1.00    8.00    --  112.00  77.00  30.00   99
 23  ω     84.00 178.00   1.00    8.00    --  112.00  30.00  90.00   94
 24  ω     79.00 178.00   1.00    8.00    --  112.00  77.00-150.00   99
 25  ω     84.00 178.00   1.00    8.00    --  112.00  30.00  60.00   94
 26  ω     84.00 178.00   1.00    8.00    --  112.00  30.00 -60.00   94
 27  ω     83.00 178.00   1.00    8.00    --  112.00  61.00-180.00   95
 28  ω     79.00 178.00   1.00    8.00    --  112.00  77.00 -30.00   99
 29  ω     86.00 178.00   1.00    8.00    --  112.00  45.00 150.00   92
 30  ω     83.00 178.00   1.00    8.00    --  112.00  61.00 -60.00   95
 31  ω     79.00 178.00   1.00    8.00    --  112.00  77.00  90.00   99
 32  ω     83.00 178.00   1.00    8.00    --  112.00  61.00-150.00   95
 33  ω     83.00 178.00   1.00    8.00    --  112.00  61.00   0.00   95
 34  ω     86.00 178.00   1.00    8.00    --  112.00  45.00  90.00   92
 35  ω     86.00 178.00   1.00    8.00    --  112.00  45.00 -30.00   92
 36  ω      1.00  82.00   1.00    4.00    --   41.22 -99.00  90.00   81
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1419345000
_diffrn_orient_matrix_UB_12      0.2435673000
_diffrn_orient_matrix_UB_13      -0.0275258000
_diffrn_orient_matrix_UB_21      0.0975195000
_diffrn_orient_matrix_UB_22      0.0839496000
_diffrn_orient_matrix_UB_23      0.1796178000
_diffrn_orient_matrix_UB_31      0.3743037000
_diffrn_orient_matrix_UB_32      -0.0977781000
_diffrn_orient_matrix_UB_33      -0.0051546000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                715
_reflns_number_total             759
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.151
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.119
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     44
_refine_ls_number_reflns         759
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0314
_refine_ls_restrained_S_all      1.096
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0539P)²+0.0338P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0806
_refine_ls_wR_factor_ref         0.0844
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B)
2.b Idealised Me refined as rotating group:
 C1(H1C,H1D,H1E)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
Cu1 Cu 0.5000 0.5000 0.5000 0.0144(2) Uani 1 2 d S T P . .
Cl1 Cl 0.04325(13) 0.22987(8) 0.36653(5) 0.0161(2) Uani 1 1 d . . . . .
O1 O 0.7531(4) 0.3666(3) 0.81213(18) 0.0190(4) Uani 1 1 d . . . . .
N1 N 0.4904(5) 0.3089(3) 0.6728(2) 0.0157(4) Uani 1 1 d . . . . .
H1A H 0.2758 0.3205 0.7027 0.019 Uiso 1 1 calc R . . . .
H1B H 0.5093 0.1561 0.6316 0.019 Uiso 1 1 calc R . . . .
C1 C 0.6720(7) 0.2258(4) 0.9260(3) 0.0198(5) Uani 1 1 d . . . . .
H1C H 0.6814 0.0591 0.8834 0.030 Uiso 1 1 calc GR . . . .
H1D H 0.4367 0.2573 0.9501 0.030 Uiso 1 1 calc GR . . . .
H1E H 0.8438 0.2669 1.0205 0.030 Uiso 1 1 calc GR . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0137(3) 0.0140(3) 0.0150(3) 0.00545(18) -0.00166(19) -0.00208(19)
Cl1 0.0147(3) 0.0153(3) 0.0175(3) 0.0028(2) -0.0001(2) -0.0014(2)
O1 0.0160(8) 0.0238(7) 0.0165(7) 0.0077(6) -0.0033(6) -0.0037(6)
N1 0.0135(9) 0.0186(8) 0.0144(8) 0.0050(6) -0.0023(7) -0.0015(7)
C1 0.0182(11) 0.0247(10) 0.0183(10) 0.0093(8) 0.0020(8) 0.0032(9)

_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
Cu1 Cl1 2.3118(6) . ?
Cu1 Cl1 2.3117(6) 2_666 ?
Cu1 N1 2.0049(17) . ?
Cu1 N1 2.0049(17) 2_666 ?
O1 N1 1.434(2) . ?
O1 C1 1.438(2) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
C1 H1C 0.9600 . ?
C1 H1D 0.9600 . ?
C1 H1E 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
Cl1 Cu1 Cl1 180.0 2_666 . ?
N1 Cu1 Cl1 83.95(5) . . ?
N1 Cu1 Cl1 83.95(5) 2_666 2_666 ?
N1 Cu1 Cl1 96.05(5) . 2_666 ?
N1 Cu1 Cl1 96.05(5) 2_666 . ?
N1 Cu1 N1 180.0 2_666 . ?
N1 O1 C1 109.20(15) . . ?
Cu1 N1 H1A 107.6 . . ?
Cu1 N1 H1B 107.6 . . ?
O1 N1 Cu1 118.86(12) . . ?
O1 N1 H1A 107.6 . . ?
O1 N1 H1B 107.6 . . ?
H1A N1 H1B 107.0 . . ?
O1 C1 H1C 109.5 . . ?
O1 C1 H1D 109.5 . . ?
O1 C1 H1E 109.5 . . ?
H1C C1 H1D 109.5 . . ?
H1C C1 H1E 109.5 . . ?
H1D C1 H1E 109.5 . . ?

_iucr_refine_instructions_details 
;

    18_pjs_019.res created by SHELXL-2014/7

TITL 18_pjs_019_a.res in P-1
REM Old TITL 18_PJS_019 in P-1 #2
REM SHELXT solution in P-1
REM R1 0.162, Rweak 0.009, Alpha 0.023, Orientation as input
REM Formula found by SHELXT: O2 Cu
CELL 1.54184 3.786793 5.68273 8.707909 99.8531 98.5632 91.5683
ZERR 1 0.000646 0.000861 0.001055 0.0115 0.012 0.013
LATT 1
SFAC Cu Cl C O N H
UNIT 1 2 2 2 2 10
 
L.S. 10
PLAN  20
SIZE 0.163 0.022 0.018
BOND $H
LIST 6
fmap 2
acta 134
REM <olex2.extras>
REM <HklSrc "%./18_PJS_019.hkl">
REM </olex2.extras>
 
WGHT    0.053900    0.033800
FVAR       1.37156
CU1   1    0.500000    0.500000    0.500000    10.50000    0.01371    0.01404 =
         0.01501    0.00545   -0.00166   -0.00208
CL1   2    0.043254    0.229866    0.366534    11.00000    0.01467    0.01529 =
         0.01747    0.00280   -0.00014   -0.00138
O1    4    0.753082    0.366639    0.812133    11.00000    0.01602    0.02377 =
         0.01655    0.00772   -0.00326   -0.00368
N1    5    0.490406    0.308884    0.672840    11.00000    0.01346    0.01864 =
         0.01436    0.00502   -0.00233   -0.00153
AFIX  23
H1A   6    0.275841    0.320539    0.702693    11.00000   -1.20000
H1B   6    0.509338    0.156128    0.631582    11.00000   -1.20000
AFIX   0
C1    3    0.671980    0.225770    0.925975    11.00000    0.01820    0.02469 =
         0.01834    0.00929    0.00204    0.00316
AFIX 137
H1C   6    0.681351    0.059088    0.883369    11.00000   -1.50000
H1D   6    0.436678    0.257254    0.950082    11.00000   -1.50000
H1E   6    0.843751    0.266898    1.020497    11.00000   -1.50000
AFIX   0
HKLF 4
 
REM  18_pjs_019_a.res in P-1
REM R1 =  0.0314 for     715 Fo > 4sig(Fo)  and  0.0331 for all     759 data
REM     44 parameters refined using      0 restraints
 
END  
     
WGHT      0.0539      0.0338 

REM Highest difference peak  1.151,  deepest hole -0.445,  1-sigma level  0.119
Q1    1   0.0000  0.5000  0.5000  10.50000  0.05    1.15
Q2    1   0.2176  0.5108  0.5055  11.00000  0.05    0.75
Q3    1   0.4639  0.7726  0.6355  11.00000  0.05    0.67
Q4    1  -0.2320  0.2576  0.3814  11.00000  0.05    0.56
Q5    1   0.2673  0.2179  0.3789  11.00000  0.05    0.48
Q6    1   0.1543  0.2632  0.5170  11.00000  0.05    0.36
Q7    1  -0.0341  0.2643  0.6151  11.00000  0.05    0.35
Q8    1   0.2239  0.3505  0.8010  11.00000  0.05    0.32
Q9    1  -0.0616  0.3895  0.4200  11.00000  0.05    0.31
Q10   1   0.3999  0.4614  0.3526  11.00000  0.05    0.31
Q11   1   0.1525  0.5172  0.4030  11.00000  0.05    0.30
Q12   1  -0.0591  0.2079  0.2471  11.00000  0.05    0.30
Q13   1   0.3469  0.1795  0.4634  11.00000  0.05    0.29
Q14   1   0.4009  0.6450  0.7189  11.00000  0.05    0.28
Q15   1   0.5000  0.0000  0.5000  10.50000  0.05    0.27
Q16   1  -0.0031  0.1534  0.2982  11.00000  0.05    0.27
Q17   1   0.8305  0.0880  0.7035  11.00000  0.05    0.26
Q18   1   0.1059  0.1018  0.4064  11.00000  0.05    0.26
Q19   1   0.8841  0.0680  0.7452  11.00000  0.05    0.25
Q20   1  -0.0178  0.2038  0.3840  11.00000  0.05    0.25

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0314 for 715 Fo > 4sig(Fo) and 0.0331 for all 3563 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 1.15, deepest hole -0.45
  REM Mean Shift 0, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0331
  REM R1_gt = 0.0314
  REM wR_ref = 0.0844
  REM GOOF = 1.096
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 3563
  REM Reflections_gt = 715
  REM Parameters = n/a
  REM Hole = -0.45
  REM Peak = 1.15
  REM Flack = n/a

  
;
_olex2_date_sample_data_collection 2017-10-25
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.416
_oxdiff_exptl_absorpt_empirical_full_min 0.788
