# Electronic Supplementary Material (ESI) for Materials Horizons.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_mo_burst135_0ma_a
_database_code_depnum_ccdc_archive 'CCDC 2068712'
loop_
_audit_author_name
_audit_author_address
'Stefan Burger'
;Technical University of Munich
Germany
;
_audit_update_record             
;
2021-03-08 deposited with the CCDC.	2021-06-14 downloaded from the CCDC.
;
_audit_creation_date             2021-03-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        C16H24N10Ni
_chemical_formula_moiety         '0.25(C24 N36 Ni4), C10 H24 N'
_chemical_formula_sum            'C16 H24 N10 Ni'
_chemical_formula_weight         415.16
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   9.8624(6)
_cell_length_b                   15.9509(9)
_cell_length_c                   12.6923(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1996.7(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9869
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.573
_cell_measurement_theta_min      2.051
_shelx_estimated_absorpt_T_max   0.850
_shelx_estimated_absorpt_T_min   0.750
_exptl_absorpt_coefficient_mu    0.995
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.7064
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0821 before and 0.0682 after correction. The Ratio of minimum to maximum transmission is 0.9470. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear greenish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             872
_exptl_crystal_preparation       
'suitable crystal selected and prepared under a microscope'
_exptl_crystal_recrystallization_method 
'mild solution approach at room temperature in water'
_exptl_crystal_size_max          0.307
_exptl_crystal_size_mid          0.202
_exptl_crystal_size_min          0.169
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_unetI/netI     0.0141
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            116055
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.573
_diffrn_reflns_theta_min         2.051
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  IMS_Mo
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          none
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2645
_reflns_number_total             2893
_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       'SAINT V8.40A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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         0.434
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.197
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         2893
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0385
_refine_ls_restrained_S_all      1.197
_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)+(0.0355P)²+2.2600P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
_refine_ls_wR_factor_ref         0.1008
_refine_special_details          none
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All H(H,H) groups, All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C10) = Uanis(C9) = Uanis(C4)
3. Others
 Fixed Sof: C6(0.5) C5(0.5) H5A(0.5) H5B(0.5) C3(0.5) C2(0.5) C7(0.5) H7A(0.5)
 H7B(0.5) C8(0.5) H8A(0.5) H8B(0.5) C1(0.5) H1A(0.5) H1B(0.5) H1C(0.5) C10(0.5)
 H10B(0.5) H10C(0.5) H10A(0.5) C9(0.5) H9A(0.5) H9B(0.5) H9C(0.5) H6A(0.5)
 H6B(0.5) H2(0.5) H3A(0.5) H3B(0.5) H3C(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C7(H7A,H7B), C8(H8A,H8B)
4.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C10(H10B,H10C,H10A), C9(H9A,H9B,H9C)
;
_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
Ni1 Ni 0.500000 0.500000 0.500000 0.01498(10) Uani 1 2 d S T P . .
N1 N 0.8895(2) 0.750000 0.49985(14) 0.0139(4) Uani 1 2 d S T P . .
N5 N 0.53793(16) 0.38545(10) 0.42916(12) 0.0210(3) Uani 1 1 d . . . . .
N4 N 0.18119(17) 0.48661(11) 0.91843(12) 0.0251(3) Uani 1 1 d . . . . .
N6 N 0.6114(3) 0.250000 0.35725(18) 0.0257(5) Uani 1 2 d S T P . .
N2 N 0.40085(17) 0.44179(10) 0.62384(13) 0.0255(3) Uani 1 1 d . . . . .
C13 C 0.56939(17) 0.32057(11) 0.39927(12) 0.0175(3) Uani 1 1 d . . . . .
C12 C 0.25705(18) 0.45410(12) 0.86257(13) 0.0207(3) Uani 1 1 d . . . . .
C11 C 0.37151(19) 0.43121(12) 0.71078(15) 0.0223(4) Uani 1 1 d . . . . .
C6 C 0.9804(4) 0.6734(2) 0.5204(3) 0.0173(6) Uani 0.5 1 d . . . A 2
C5 C 0.9223(4) 0.6788(2) 0.5735(3) 0.0180(6) Uani 0.5 1 d . . . A 1
H5A H 0.863949 0.630435 0.555178 0.022 Uiso 0.5 1 calc R . . A 1
H5B H 0.898894 0.696131 0.646124 0.022 Uiso 0.5 1 calc R . . A 1
C3 C 0.8583(4) 0.7806(2) 0.3018(3) 0.0183(6) Uani 0.5 1 d . . . . .
C2 C 0.9107(3) 0.7780(2) 0.3869(3) 0.0171(6) Uani 0.5 1 d . . . A .
C7 C 1.0689(4) 0.6501(2) 0.5723(3) 0.0224(7) Uani 0.5 1 d . . . A 1
H7A H 1.128658 0.698145 0.588808 0.027 Uiso 0.5 1 calc R . . A 1
H7B H 1.092362 0.629733 0.500845 0.027 Uiso 0.5 1 calc R . . A 1
C8 C 0.9849(4) 0.6424(2) 0.6329(3) 0.0226(7) Uani 0.5 1 d . . . A 2
H8A H 0.892816 0.626774 0.656971 0.027 Uiso 0.5 1 calc R . . A 2
H8B H 1.020494 0.686671 0.679975 0.027 Uiso 0.5 1 calc R . . A 2
C1 C 0.7437(3) 0.7740(2) 0.5165(3) 0.0207(7) Uani 0.5 1 d . . . A -1
H1A H 0.685124 0.726746 0.497548 0.031 Uiso 0.5 1 calc GR . . A -1
H1B H 0.721553 0.822395 0.472111 0.031 Uiso 0.5 1 calc GR . . A -1
H1C H 0.729403 0.788598 0.590671 0.031 Uiso 0.5 1 calc GR . . A -1
C10 C 1.0790(8) 0.5652(4) 0.6348(5) 0.0249(5) Uani 0.5 1 d . . . A 2
H10B H 1.044533 0.522698 0.585930 0.037 Uiso 0.5 1 calc GR . . A 2
H10C H 1.081684 0.541944 0.706261 0.037 Uiso 0.5 1 calc GR . . A 2
H10A H 1.170606 0.581921 0.613527 0.037 Uiso 0.5 1 calc GR . . A 2
C9 C 1.0933(8) 0.5802(4) 0.6520(4) 0.0249(5) Uani 0.5 1 d . . . A 1
H9A H 1.071394 0.600444 0.722846 0.037 Uiso 0.5 1 calc GR . . A 1
H9B H 1.188760 0.563144 0.649474 0.037 Uiso 0.5 1 calc GR . . A 1
H9C H 1.035620 0.532078 0.634850 0.037 Uiso 0.5 1 calc GR . . A 1
C4 C 0.9127(3) 0.750000 0.1947(2) 0.0249(5) Uani 1 2 d S T P A .
N3 N 0.34752(18) 0.41215(12) 0.80937(13) 0.0298(4) Uani 1 1 d . . . . .
H6A H 1.085(6) 0.687(4) 0.498(4) 0.036 Uiso 0.5 1 d R . . B 2
H6B H 0.944(6) 0.631(4) 0.476(4) 0.036 Uiso 0.5 1 d R . . C 2
H2 H 1.010(4) 0.788(3) 0.376(4) 0.023(12) Uiso 0.5 1 d . . . . .
H3A H 0.768(5) 0.781(3) 0.302(4) 0.033(14) Uiso 0.5 1 d . . . . .
H3B H 0.862(4) 0.840(3) 0.381(4) 0.016(10) Uiso 0.5 1 d . . . . .
H3C H 0.883(5) 0.838(3) 0.314(4) 0.025(12) Uiso 0.5 1 d . . . . .
H4A H 1.017(4) 0.750000 0.195(3) 0.037 Uiso 1 2 d RS T P . .
H4B H 0.883(3) 0.7044(16) 0.157(2) 0.037 Uiso 1 1 d R . . . .


_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
Ni1 N5 2.0705(16) 5_666 ?
Ni1 N5 2.0705(16) . ?
Ni1 N4 2.0763(16) 2_564 ?
Ni1 N4 2.0763(16) 6_657 ?
Ni1 N2 2.0709(15) . ?
Ni1 N2 2.0710(15) 5_666 ?
N1 C6 1.538(4) . ?
N1 C6 1.538(4) 7_575 ?
N1 C5 1.506(3) 7_575 ?
N1 C5 1.506(3) . ?
N1 C2 1.516(4) . ?
N1 C2 1.516(4) 7_575 ?
N1 C1 1.503(4) . ?
N5 C13 1.145(2) . ?
N4 C12 1.154(2) . ?
N6 C13 1.313(2) . ?
N6 C13 1.313(2) 7_565 ?
N2 C11 1.153(2) . ?
C12 N3 1.304(2) . ?
C11 N3 1.309(2) . ?
C6 C2 1.986(5) 7_575 ?
C6 C8 1.511(5) . ?
C5 C7 1.516(5) . ?
C3 C3 0.975(7) 7_575 ?
C3 C2 1.518(5) 7_575 ?
C3 C2 1.198(5) . ?
C3 C4 1.541(4) . ?
C2 C2 0.893(7) 7_575 ?
C7 C9 1.524(7) . ?
C8 C10 1.542(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N5 Ni1 N5 180.0 5_666 . ?
N5 Ni1 N4 91.70(6) . 2_564 ?
N5 Ni1 N4 88.30(6) . 6_657 ?
N5 Ni1 N4 88.30(6) 5_666 2_564 ?
N5 Ni1 N4 91.70(6) 5_666 6_657 ?
N5 Ni1 N2 88.90(6) 5_666 . ?
N5 Ni1 N2 91.10(6) 5_666 5_666 ?
N5 Ni1 N2 88.90(6) . 5_666 ?
N5 Ni1 N2 91.10(6) . . ?
N4 Ni1 N4 180.0 2_564 6_657 ?
N2 Ni1 N4 91.04(7) 5_666 6_657 ?
N2 Ni1 N4 91.04(7) . 2_564 ?
N2 Ni1 N4 88.96(7) 5_666 2_564 ?
N2 Ni1 N4 88.96(7) . 6_657 ?
N2 Ni1 N2 180.0 . 5_666 ?
C5 N1 C6 33.90(18) 7_575 7_575 ?
C5 N1 C6 111.6(2) . 7_575 ?
C5 N1 C5 97.9(3) 7_575 . ?
C5 N1 C2 109.56(19) . 7_575 ?
C5 N1 C2 109.56(19) 7_575 . ?
C5 N1 C2 141.2(2) . . ?
C5 N1 C2 141.2(2) 7_575 7_575 ?
C2 N1 C6 108.3(2) . . ?
C2 N1 C6 108.3(2) 7_575 7_575 ?
C2 N1 C6 81.1(2) . 7_575 ?
C2 N1 C6 81.1(2) 7_575 . ?
C2 N1 C2 34.2(3) . 7_575 ?
C1 N1 C6 109.3(2) . 7_575 ?
C1 N1 C5 85.8(2) . 7_575 ?
C1 N1 C5 108.1(2) . . ?
C1 N1 C2 101.0(2) . . ?
C1 N1 C2 109.9(2) . 7_575 ?
C13 N5 Ni1 172.06(15) . . ?
C12 N4 Ni1 155.61(17) . 2_565 ?
C13 N6 C13 118.1(2) . 7_565 ?
C11 N2 Ni1 155.55(18) . . ?
N5 C13 N6 174.33(18) . . ?
N4 C12 N3 173.04(19) . . ?
N2 C11 N3 173.6(2) . . ?
N1 C6 C2 48.96(15) . 7_575 ?
C8 C6 N1 116.0(3) . . ?
C8 C6 C2 160.7(3) . 7_575 ?
N1 C5 C7 115.3(3) . . ?
C3 C3 C2 88.0(2) 7_575 . ?
C3 C3 C2 52.03(19) 7_575 7_575 ?
C3 C3 C4 71.55(14) 7_575 . ?
C2 C3 C2 36.0(3) . 7_575 ?
C2 C3 C4 129.4(3) . . ?
C2 C3 C4 108.3(3) 7_575 . ?
N1 C2 C6 49.90(15) . 7_575 ?
N1 C2 C3 116.4(3) . 7_575 ?
C3 C2 N1 143.4(3) . . ?
C3 C2 C6 164.7(3) 7_575 7_575 ?
C3 C2 C6 154.8(3) . 7_575 ?
C3 C2 C3 39.9(3) . 7_575 ?
C2 C2 N1 72.88(13) 7_575 . ?
C2 C2 C6 112.98(15) 7_575 7_575 ?
C2 C2 C3 92.0(2) 7_575 . ?
C2 C2 C3 52.03(19) 7_575 7_575 ?
C5 C7 C9 111.4(4) . . ?
C6 C8 C10 107.1(3) . . ?
C3 C4 C3 36.9(3) 7_575 . ?
C12 N3 C11 119.96(16) . . ?

_olex2_exptl_crystal_mounting_method 
'suitable piece of crystal selected in perfluoroether oil and mounted on top of a microloop sample holder'
_olex2_submission_original_sample_id BurSt135
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_mo_burst117_0m_b
_database_code_depnum_ccdc_archive 'CCDC 2068844'
loop_
_audit_author_name
_audit_author_address
'Stefan Burger'
;Technical University of Munich
Germany
;
_audit_update_record             
;
2021-03-08 deposited with the CCDC.	2021-06-14 downloaded from the CCDC.
;
_audit_creation_date             2021-03-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        C16H24N10Ni
_chemical_formula_moiety         '0.17(C36 N54 Ni6), C10 H24 N1'
_chemical_formula_sum            'C16 H24 N10 Ni'
_chemical_formula_weight         415.16
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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      trigonal
_space_group_IT_number           161
_space_group_name_H-M_alt        'R 3 c'
_space_group_name_Hall           'R 3 -2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'

_cell_length_a                   12.5883(8)
_cell_length_b                   12.5883(8)
_cell_length_c                   21.565(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2959.5(5)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    9885
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.575
_cell_measurement_theta_min      2.657
_shelx_estimated_absorpt_T_max   0.856
_shelx_estimated_absorpt_T_min   0.743
_exptl_absorpt_coefficient_mu    1.007
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.7090
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0560 before and 0.0464 after correction. The Ratio of minimum to maximum transmission is 0.9503. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear greenish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1308
_exptl_crystal_preparation       
'appropriate crystal prepared in perfluoroether oil'
_exptl_crystal_recrystallization_method 
'high entropy crystallisation from water precursor solution at 95 degree C'
_exptl_crystal_size_max          0.314
_exptl_crystal_size_mid          0.277
_exptl_crystal_size_min          0.16
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            16219
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.575
_diffrn_reflns_theta_min         2.657
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  IMS_Mo
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          none
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.992
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                1783
_reflns_number_total             1840
_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       'SAINT V8.40A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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         0.199
_refine_diff_density_min         -0.236
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.443(15)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     87
_refine_ls_number_reflns         1840
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0173
_refine_ls_R_factor_gt           0.0161
_refine_ls_restrained_S_all      1.047
_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)+(0.0200P)²+1.7882P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0401
_refine_ls_wR_factor_ref         0.0408
_refine_special_details          none,Twin
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.557(16)
 0.443(16)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C4(H4A,H4B)
3.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C)
;
_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
Ni1 Ni 0.333333 0.666667 0.64236(2) 0.00919(8) Uani 1 3 d S T P . .
N4 N 0.13381(13) 0.14240(13) 0.52872(7) 0.0164(3) Uani 1 1 d . . . . .
N2 N 0.32016(13) 0.52634(12) 0.58732(7) 0.0149(3) Uani 1 1 d . . . . .
N1 N 0.666667 0.333333 0.54854(10) 0.0122(6) Uani 1 3 d S T P . .
N3 N 0.31141(13) 0.35169(13) 0.53177(7) 0.0231(3) Uani 1 1 d . . . . .
C2 C 0.21371(14) 0.24231(14) 0.53160(7) 0.0144(3) Uani 1 1 d . . . . .
C1 C 0.30977(13) 0.44086(14) 0.56242(7) 0.0138(3) Uani 1 1 d . . . . .
C3 C 0.666667 0.333333 0.61837(14) 0.0206(6) Uani 1 3 d S T P . .
C5 C 0.70749(15) 0.55407(14) 0.53728(8) 0.0202(3) Uani 1 1 d . . . . .
H5A H 0.778987 0.586353 0.509049 0.024 Uiso 1 1 calc R . . . .
H5B H 0.738000 0.565596 0.580468 0.024 Uiso 1 1 calc R . . . .
C4 C 0.62212(14) 0.41801(14) 0.52464(8) 0.0159(3) Uani 1 1 d . . . . .
H4A H 0.541479 0.393137 0.543730 0.019 Uiso 1 1 calc R . . . .
H4B H 0.609436 0.406107 0.479304 0.019 Uiso 1 1 calc R . . . .
C6 C 0.63893(16) 0.62429(15) 0.52736(9) 0.0241(3) Uani 1 1 d . . . . .
H6A H 0.602193 0.606425 0.485884 0.036 Uiso 1 1 calc GR . . . .
H6B H 0.696406 0.712522 0.531193 0.036 Uiso 1 1 calc GR . . . .
H6C H 0.574216 0.598947 0.558633 0.036 Uiso 1 1 calc GR . . . .
H3 H 0.728(2) 0.408(3) 0.6336(13) 0.036 Uiso 1 1 d R . . . .


_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
Ni1 N4 2.0828(15) 17_554 ?
Ni1 N4 2.0829(15) 16_554 ?
Ni1 N4 2.0829(15) 18_554 ?
Ni1 N2 2.0650(14) 3_565 ?
Ni1 N2 2.0650(14) 2_665 ?
Ni1 N2 2.0650(14) . ?
N4 C2 1.154(2) . ?
N2 C1 1.150(2) . ?
N1 C3 1.506(3) . ?
N1 C4 1.5211(17) 2_655 ?
N1 C4 1.5211(17) . ?
N1 C4 1.5211(17) 3_665 ?
N3 C2 1.310(2) . ?
N3 C1 1.312(2) . ?
C3 H3 0.93(3) 2_655 ?
C3 H3 0.93(3) 3_665 ?
C3 H3 0.93(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C4 1.524(2) . ?
C5 C6 1.528(2) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?

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
N4 Ni1 N4 92.75(6) 16_554 18_554 ?
N4 Ni1 N4 92.76(6) 17_554 16_554 ?
N4 Ni1 N4 92.75(6) 17_554 18_554 ?
N2 Ni1 N4 89.55(6) 3_565 16_554 ?
N2 Ni1 N4 177.67(7) 3_565 18_554 ?
N2 Ni1 N4 177.67(7) . 17_554 ?
N2 Ni1 N4 87.43(6) 2_665 18_554 ?
N2 Ni1 N4 89.55(6) 2_665 17_554 ?
N2 Ni1 N4 87.43(6) 3_565 17_554 ?
N2 Ni1 N4 87.43(6) . 16_554 ?
N2 Ni1 N4 177.67(7) 2_665 16_554 ?
N2 Ni1 N4 89.55(6) . 18_554 ?
N2 Ni1 N2 90.25(6) . 2_665 ?
N2 Ni1 N2 90.25(6) 3_565 2_665 ?
N2 Ni1 N2 90.25(6) 3_565 . ?
C2 N4 Ni1 148.91(13) . 10_554 ?
C1 N2 Ni1 172.64(13) . . ?
C3 N1 C4 109.80(10) . . ?
C3 N1 C4 109.80(11) . 2_655 ?
C3 N1 C4 109.80(11) . 3_665 ?
C4 N1 C4 109.14(11) 3_665 2_655 ?
C4 N1 C4 109.14(11) 2_655 . ?
C4 N1 C4 109.14(11) 3_665 . ?
C2 N3 C1 119.53(14) . . ?
N4 C2 N3 173.93(18) . . ?
N2 C1 N3 173.17(17) . . ?
N1 C3 H3 110.7(17) . 3_665 ?
N1 C3 H3 110.7(17) . . ?
N1 C3 H3 110.7(17) . 2_655 ?
H3 C3 H3 108.2(18) . 3_665 ?
H3 C3 H3 108.2(18) 2_655 3_665 ?
H3 C3 H3 108.2(18) . 2_655 ?
H5A C5 H5B 108.2 . . ?
C4 C5 H5A 109.7 . . ?
C4 C5 H5B 109.7 . . ?
C4 C5 C6 109.89(13) . . ?
C6 C5 H5A 109.7 . . ?
C6 C5 H5B 109.7 . . ?
N1 C4 C5 115.29(12) . . ?
N1 C4 H4A 108.5 . . ?
N1 C4 H4B 108.5 . . ?
C5 C4 H4A 108.5 . . ?
C5 C4 H4B 108.5 . . ?
H4A C4 H4B 107.5 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?

_olex2_exptl_crystal_mounting_method 'mounted on microloop sample holder'
_olex2_submission_original_sample_id BurSt117
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.557(16)
2 0.443(16)

####################################################################### 
# 
# 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_mo_burst199_0m_b
_database_code_depnum_ccdc_archive 'CCDC 2068846'
loop_
_audit_author_name
_audit_author_address
'Stefan Burger'
;Technical University of Munich
Germany
;
_audit_update_record             
;
2021-03-08 deposited with the CCDC.	2021-06-14 downloaded from the CCDC.
;
_audit_creation_date             2021-03-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        C16H24N10Co
_chemical_formula_moiety         '0.17(C36 Co6 N54), 1(C10 H24 N1)'
_chemical_formula_sum            'C16 H24 Co N10'
_chemical_formula_weight         415.38
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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'

_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      trigonal
_space_group_IT_number           161
_space_group_name_H-M_alt        'R 3 c'
_space_group_name_Hall           'R 3 -2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'

_cell_length_a                   12.6783(16)
_cell_length_b                   12.6783(16)
_cell_length_c                   21.585(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3004.7(10)
_cell_formula_units_Z            5.99994
_cell_measurement_reflns_used    9882
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.277
_cell_measurement_theta_min      2.646
_shelx_estimated_absorpt_T_max   0.858
_shelx_estimated_absorpt_T_min   0.813
_exptl_absorpt_coefficient_mu    0.880
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.7131
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0599 before and 0.0425 after correction. The Ratio of minimum to maximum transmission is 0.9560. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear pinkish pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   pinkish
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             1302
_exptl_crystal_preparation       'crystal prepared in perfluoro ether oil'
_exptl_crystal_recrystallization_method 'mild solution approach'
_exptl_crystal_size_max          0.246
_exptl_crystal_size_mid          0.204
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_unetI/netI     0.0148
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            15254
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.277
_diffrn_reflns_theta_min         2.646
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  TXS
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          none
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.990
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                1590
_reflns_number_total             1650
_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       'SAINT V8.40A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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         0.173
_refine_diff_density_min         -0.166
_refine_diff_density_rms         0.035
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.448(19)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     87
_refine_ls_number_reflns         1650
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0183
_refine_ls_R_factor_gt           0.0166
_refine_ls_restrained_S_all      1.090
_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)+(0.0193P)²+2.0713P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0410
_refine_ls_wR_factor_ref         0.0429
_refine_special_details          none,Twin
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.552(19)
 0.448(19)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B)
3.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C)
;
_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
Co1 Co 0.333333 0.666667 0.64219(3) 0.01062(9) Uani 1 3 d S T P . .
N1 N 0.666667 0.333333 0.54899(14) 0.0134(8) Uani 1 3 d S T P . .
N4 N 0.13669(15) 0.14341(15) 0.52925(8) 0.0189(4) Uani 1 1 d . . . . .
N3 N 0.31372(15) 0.35103(15) 0.53187(9) 0.0266(4) Uani 1 1 d . . . . .
N2 N 0.32189(15) 0.52520(14) 0.58616(8) 0.0168(3) Uani 1 1 d . . . . .
C2 C 0.21641(17) 0.24250(17) 0.53193(9) 0.0162(4) Uani 1 1 d . . . . .
C1 C 0.31187(16) 0.44013(16) 0.56184(9) 0.0155(3) Uani 1 1 d . . . . .
C4 C 0.62243(16) 0.41766(16) 0.52503(9) 0.0185(4) Uani 1 1 d . . . . .
H4A H 0.609883 0.405869 0.479728 0.022 Uiso 1 1 calc R . . . .
H4B H 0.542359 0.393046 0.544079 0.022 Uiso 1 1 calc R . . . .
C5 C 0.70742(17) 0.55277(16) 0.53771(10) 0.0228(4) Uani 1 1 d . . . . .
H5A H 0.778493 0.584680 0.509569 0.027 Uiso 1 1 calc R . . . .
H5B H 0.737558 0.564087 0.580882 0.027 Uiso 1 1 calc R . . . .
C3 C 0.666667 0.333333 0.61859(17) 0.0239(7) Uani 1 3 d S T P . .
C6 C 0.63976(19) 0.62292(18) 0.52772(11) 0.0271(4) Uani 1 1 d . . . . .
H6A H 0.603795 0.605698 0.486173 0.041 Uiso 1 1 calc GR . . . .
H6B H 0.696956 0.710449 0.531822 0.041 Uiso 1 1 calc GR . . . .
H6C H 0.575141 0.597598 0.558775 0.041 Uiso 1 1 calc GR . . . .
H3 H 0.731(3) 0.414(3) 0.6337(14) 0.041 Uiso 1 1 d R . . . .


_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 N4 2.1220(18) 16_554 ?
Co1 N4 2.1220(18) 18_554 ?
Co1 N4 2.1219(18) 17_554 ?
Co1 N2 2.1073(17) 3_565 ?
Co1 N2 2.1072(17) . ?
Co1 N2 2.1073(17) 2_665 ?
N1 C4 1.525(2) 2_655 ?
N1 C4 1.525(2) . ?
N1 C4 1.525(2) 3_665 ?
N1 C3 1.502(4) . ?
N4 C2 1.155(3) . ?
N3 C2 1.311(3) . ?
N3 C1 1.312(2) . ?
N2 C1 1.148(2) . ?
C4 C5 1.525(3) . ?
C5 C6 1.529(3) . ?

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
N4 Co1 N4 92.98(7) 16_554 18_554 ?
N4 Co1 N4 92.98(7) 17_554 18_554 ?
N4 Co1 N4 92.98(7) 17_554 16_554 ?
N2 Co1 N4 89.40(7) 3_565 16_554 ?
N2 Co1 N4 87.27(7) 2_665 18_554 ?
N2 Co1 N4 89.40(7) 2_665 17_554 ?
N2 Co1 N4 177.58(8) 2_665 16_554 ?
N2 Co1 N4 89.40(7) . 18_554 ?
N2 Co1 N4 87.27(7) 3_565 17_554 ?
N2 Co1 N4 177.59(8) . 17_554 ?
N2 Co1 N4 177.59(8) 3_565 18_554 ?
N2 Co1 N4 87.27(7) . 16_554 ?
N2 Co1 N2 90.33(7) 2_665 . ?
N2 Co1 N2 90.33(7) 3_565 . ?
N2 Co1 N2 90.33(7) 3_565 2_665 ?
C4 N1 C4 109.12(14) 3_665 2_655 ?
C4 N1 C4 109.11(14) 2_655 . ?
C4 N1 C4 109.11(14) 3_665 . ?
C3 N1 C4 109.83(14) . . ?
C3 N1 C4 109.83(14) . 3_665 ?
C3 N1 C4 109.83(14) . 2_655 ?
C2 N4 Co1 148.78(16) . 10_554 ?
C2 N3 C1 119.38(16) . . ?
C1 N2 Co1 171.99(16) . . ?
N4 C2 N3 174.0(2) . . ?
N2 C1 N3 173.2(2) . . ?
C5 C4 N1 115.20(14) . . ?
C4 C5 C6 109.96(16) . . ?

_olex2_exptl_crystal_mounting_method 'mounted on microloop sample holder'
_olex2_submission_original_sample_id C16H24N10Co
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.552(19)
2 0.448(19)

####################################################################### 
# 
# 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_mo_burst118_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2068845'
loop_
_audit_author_name
_audit_author_address
'Stefan Burger'
;Technical University of Munich
Germany
;
_audit_update_record             
;
2021-03-08 deposited with the CCDC.	2021-06-14 downloaded from the CCDC.
;
_audit_creation_date             2021-03-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        C16H24N10Ni
_chemical_formula_moiety         '0.17(C36 N54 Ni6), 1(C9 H21 N1), 2(C0.5 H1.5)'
_chemical_formula_sum            'C16 H24 N10 Ni'
_chemical_formula_weight         415.15
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c'
_space_group_name_Hall           '-R 3 2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   12.5350(3)
_cell_length_b                   12.5350(3)
_cell_length_c                   22.8074(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3103.5(2)
_cell_formula_units_Z            6.00012
_cell_measurement_reflns_used    9955
_cell_measurement_temperature    350(2)
_cell_measurement_theta_max      27.868
_cell_measurement_theta_min      2.591
_shelx_estimated_absorpt_T_max   0.862
_shelx_estimated_absorpt_T_min   0.753
_exptl_absorpt_coefficient_mu    0.960
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.7084
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0426 before and 0.0382 after correction. The Ratio of minimum to maximum transmission is 0.9500. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear greenish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1308
_exptl_crystal_preparation       
'appropriate crystal prepared in perfluoroether oil'
_exptl_crystal_recrystallization_method 
'high entropy crystallisation from water precursor solution at 95 degree C'
_exptl_crystal_size_max          0.314
_exptl_crystal_size_mid          0.277
_exptl_crystal_size_min          0.16
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_av_unetI/netI     0.0079
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            17980
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.868
_diffrn_reflns_theta_min         2.590
_diffrn_ambient_temperature      350.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  IMS_Mo
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          none
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                740
_reflns_number_total             830
_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       'SAINT V8.40A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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         0.157
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.036
_refine_ls_extinction_coef       0.0018(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     103
_refine_ls_number_reflns         830
_refine_ls_number_restraints     84
_refine_ls_R_factor_all          0.0261
_refine_ls_R_factor_gt           0.0234
_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)+(0.0432P)²+0.9516P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0656
_refine_ls_wR_factor_ref         0.0691
_refine_special_details          none
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All N(H) groups
2. Uiso/Uaniso restraints and constraints
C3 \\sim C4 \\sim C5 \\sim C5A \\sim C4A \\sim C3A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C3A) = Uanis(C2)
3. Rigid body (RIGU) restrains
 C3, C4, C5, C5A, C4A, C3A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Others
 Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(C5A)=Sof(H5AA)=
 Sof(H5AB)=Sof(H5AC)=0.5*(1-FVAR(2))
 Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C5)=Sof(H5A)=Sof(H5B)=
 Sof(H5C)=0.5*FVAR(2)
 Fixed Sof: C2(0.16667) N3(0.4) N3A(0.1) H2(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C3(H3A,H3B), C3A(H3AA,H3AB), C4A(H4AA,H4AB)
5.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C5A(H5AA,H5AB,H5AC)
;
_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
Ni1 Ni 0.666667 0.333333 0.333333 0.04092(17) Uani 1 6 d S T P . .
N2 N 0.52306(10) 0.31868(10) 0.38468(6) 0.0641(3) Uani 1 1 d . . . . .
N1 N 0.666667 0.333333 0.583333 0.0670(9) Uani 1 6 d S T P . .
C1 C 0.43194(12) 0.30578(11) 0.40006(7) 0.0610(4) Uani 1 1 d . . . . .
C4 C 0.4847(6) 0.3744(7) 0.5984(5) 0.086(2) Uani 0.315(6) 1 d . U . A -2
H4A H 0.545318 0.444275 0.575965 0.104 Uiso 0.315(6) 1 calc R . . A -2
H4B H 0.487186 0.405464 0.637604 0.104 Uiso 0.315(6) 1 calc R . . A -2
C3 C 0.5383(7) 0.2945(8) 0.6047(5) 0.090(2) Uani 0.315(6) 1 d . U . A -2
H3A H 0.482851 0.217420 0.585301 0.108 Uiso 0.315(6) 1 calc R . . A -2
H3B H 0.536066 0.276049 0.646174 0.108 Uiso 0.315(6) 1 calc R . . A -2
C3A C 0.5725(16) 0.365(2) 0.6049(10) 0.114(3) Uani 0.185(6) 1 d . U . A -3
H3AA H 0.522660 0.306629 0.634939 0.137 Uiso 0.185(6) 1 calc R . . A -3
H3AB H 0.615027 0.446254 0.622863 0.137 Uiso 0.185(6) 1 calc R . . A -3
C4A C 0.4910(14) 0.3652(18) 0.5587(10) 0.110(3) Uani 0.185(6) 1 d . U . A -3
H4AA H 0.544887 0.436856 0.535340 0.131 Uiso 0.185(6) 1 calc R . . A -3
H4AB H 0.475111 0.294850 0.534749 0.131 Uiso 0.185(6) 1 calc R . . A -3
C5 C 0.3649(16) 0.3493(18) 0.5745(11) 0.099(5) Uani 0.315(6) 1 d . U . A -2
H5A H 0.376784 0.384672 0.536005 0.148 Uiso 0.315(6) 1 calc GR . . A -2
H5B H 0.329923 0.385140 0.599681 0.148 Uiso 0.315(6) 1 calc GR . . A -2
H5C H 0.310202 0.261974 0.572139 0.148 Uiso 0.315(6) 1 calc GR . . A -2
C5A C 0.389(2) 0.364(3) 0.5579(14) 0.109(6) Uani 0.185(6) 1 d . U . A -3
H5AA H 0.322257 0.280415 0.556658 0.164 Uiso 0.185(6) 1 calc GR . . A -3
H5AB H 0.385523 0.407377 0.523905 0.164 Uiso 0.185(6) 1 calc GR . . A -3
H5AC H 0.381784 0.403478 0.592608 0.164 Uiso 0.185(6) 1 calc GR . . A -3
C2 C 0.666667 0.333333 0.6522(6) 0.114(3) Uani 0.5 3 d S T P A 1
N3 N 0.3429(14) 0.3117(10) 0.4274(5) 0.054(7) Uani 0.4 1 d . . . B 1
N3A N 0.364(3) 0.312(3) 0.447(2) 0.060(10) Uani 0.1 1 d . . . B 2
H2 H 0.772(5) 0.388(3) 0.654(2) 0.089 Uiso 0.5 1 d R . . . .


_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
Ni1 N2 2.0773(11) 31_655 ?
Ni1 N2 2.0773(11) 3_665 ?
Ni1 N2 2.0773(11) 2_655 ?
Ni1 N2 2.0773(11) 33_545 ?
Ni1 N2 2.0772(11) 32 ?
Ni1 N2 2.0772(11) . ?
N2 C1 1.1266(16) . ?
N1 C3 1.511(6) . ?
N1 C3A 1.506(19) . ?
N1 C2 1.570(14) 16_545 ?
N1 C2 1.570(14) . ?
C1 N3 1.313(13) . ?
C1 N3 1.341(15) 12 ?
C1 N3A 1.40(4) . ?
C1 N3A 1.53(4) 12 ?
C4 C3 1.465(10) . ?
C4 C5 1.48(2) . ?
C3A C4A 1.47(3) . ?
C4A C5A 1.27(3) . ?
N3 N3 0.53(2) 12 ?
N3A N3A 1.55(10) 12 ?

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
N2 Ni1 N2 91.33(5) 31_655 33_545 ?
N2 Ni1 N2 91.33(5) 2_655 . ?
N2 Ni1 N2 91.33(5) 2_655 3_665 ?
N2 Ni1 N2 91.33(5) 31_655 32 ?
N2 Ni1 N2 180.0 33_545 3_665 ?
N2 Ni1 N2 91.33(5) 33_545 32 ?
N2 Ni1 N2 88.67(5) 33_545 . ?
N2 Ni1 N2 88.67(5) 31_655 2_655 ?
N2 Ni1 N2 88.67(5) 31_655 3_665 ?
N2 Ni1 N2 88.67(5) 33_545 2_655 ?
N2 Ni1 N2 88.67(5) 32 3_665 ?
N2 Ni1 N2 180.0 32 2_655 ?
N2 Ni1 N2 91.33(5) . 3_665 ?
N2 Ni1 N2 180.0 31_655 . ?
N2 Ni1 N2 88.67(5) 32 . ?
C1 N2 Ni1 163.71(13) . . ?
C2 N1 C2 180.0 16_545 . ?
N2 C1 N3 166.3(5) . 12 ?
N2 C1 N3 165.8(6) . . ?
N2 C1 N3A 149.6(18) . 12 ?
N2 C1 N3A 146.4(19) . . ?
N3 C1 N3 23.2(9) . 12 ?
N3 C1 N3A 19.8(15) 12 12 ?
N3 C1 N3A 43(2) . 12 ?
N3A C1 N3A 64(4) . 12 ?
C3 C4 C5 131.0(11) . . ?
C4 C3 N1 121.7(7) . . ?
C4A C3A N1 113.8(17) . . ?
C5A C4A C3A 135(2) . . ?
C1 N3 C1 117.7(7) . 12 ?
N3 N3 C1 81(3) 12 . ?
N3 N3 C1 75(3) 12 12 ?
C1 N3A C1 102(3) . 12 ?
C1 N3A N3A 54(2) 12 12 ?
C1 N3A N3A 62(3) . 12 ?

_olex2_exptl_crystal_mounting_method 'mounted on microloop sample holder'
_olex2_submission_original_sample_id BurSt118
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_burst128_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2068849'
loop_
_audit_author_name
_audit_author_address
'Stefan Burger'
;Technical University of Munich
Germany
;
_audit_update_record             
;
2021-03-08 deposited with the CCDC.	2021-06-14 downloaded from the CCDC.
;
_audit_creation_date             2021-03-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        C16H24N10Mn
_chemical_formula_moiety         '0.17(C36 Mn6 N54), 1(C9 H21 N1), 2(C0.5 H1.5)'
_chemical_formula_sum            'C16 H24 Mn N10'
_chemical_formula_weight         411.38
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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'

_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      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c'
_space_group_name_Hall           '-R 3 2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   12.7694(5)
_cell_length_b                   12.7694(5)
_cell_length_c                   23.0222(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3251.0(3)
_cell_formula_units_Z            6.00012
_cell_measurement_reflns_used    9994
_cell_measurement_temperature    350(2)
_cell_measurement_theta_max      29.56
_cell_measurement_theta_min      2.554
_shelx_estimated_absorpt_T_max   0.928
_shelx_estimated_absorpt_T_min   0.892
_exptl_absorpt_coefficient_mu    0.630
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.7097
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0881 before and 0.0493 after correction. The Ratio of minimum to maximum transmission is 0.9512. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1290
_exptl_crystal_preparation       
'suitable crystal was prepared in perfluoroether oil under a microscope'
_exptl_crystal_recrystallization_method 
'high entropy crystallisation from water precursor solution at 95 degree C'
_exptl_crystal_size_max          0.185
_exptl_crystal_size_mid          0.169
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_unetI/netI     0.0124
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            57844
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.560
_diffrn_reflns_theta_min         2.554
_diffrn_ambient_temperature      350.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  TXS
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          none
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                780
_reflns_number_total             1025
_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       'SAINT V8.40A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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         0.159
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         1025
_refine_ls_number_restraints     63
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0391
_refine_ls_restrained_S_all      1.076
_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)+(0.0756P)²+0.9390P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1197
_refine_ls_wR_factor_ref         0.1317
_refine_special_details          none
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C3 \\sim C4 \\sim C5 \\sim C4A \\sim C3A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C5) = Uanis(C5A)
3. Rigid body (RIGU) restrains
 C3, C4, C5, C4A, C3A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Same fragment restrains
{C3, C4, C5} sigma for 1-2: 0.01, 1-3: 0.04
as
{C3A, C4A, C5A}
5. Others
 Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(C5A)=Sof(H5AA)=
 Sof(H5AB)=Sof(H5AC)=0.5*(1-FVAR(2))
 Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C5)=Sof(H5A)=Sof(H5B)=
 Sof(H5C)=0.5*FVAR(2)
 Fixed Sof: N3B(0.15) N3A(0.35) C2(0.16667) H2(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C3(H3A,H3B), C3A(H3AA,H3AB), C4A(H4AA,H4AB)
6.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C5A(H5AA,H5AB,H5AC)
;
_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 0.666667 0.333333 0.333333 0.0651(3) Uani 1 6 d S T P . .
N2 N 0.67575(17) 0.48078(16) 0.38742(9) 0.1060(6) Uani 1 1 d . . . . .
C1 C 0.68864(17) 0.56920(18) 0.40204(10) 0.0912(6) Uani 1 1 d . . . . .
N1 N 0.666667 0.333333 0.583333 0.0921(13) Uani 1 6 d S T P . .
C4 C 0.7034(12) 0.5497(10) 0.5666(6) 0.117(3) Uani 0.323(8) 1 d D U . A -2
H4A H 0.634174 0.510769 0.540865 0.140 Uiso 0.323(8) 1 calc R . . A -2
H4B H 0.775906 0.587912 0.542895 0.140 Uiso 0.323(8) 1 calc R . . A -2
C3 C 0.7065(13) 0.4611(10) 0.6032(6) 0.116(3) Uani 0.323(8) 1 d D U . A -2
H3A H 0.658300 0.453749 0.637194 0.139 Uiso 0.323(8) 1 calc R . . A -2
H3B H 0.789292 0.495339 0.616568 0.139 Uiso 0.323(8) 1 calc R . . A -2
C5 C 0.6952(18) 0.6462(15) 0.6029(11) 0.137(4) Uani 0.323(8) 1 d D U . A -2
H5A H 0.727417 0.649547 0.640933 0.205 Uiso 0.323(8) 1 calc GR . . A -2
H5B H 0.612212 0.625851 0.605992 0.205 Uiso 0.323(8) 1 calc GR . . A -2
H5C H 0.740987 0.723508 0.584311 0.205 Uiso 0.323(8) 1 calc GR . . A -2
C3A C 0.699(2) 0.4534(17) 0.5637(10) 0.113(4) Uani 0.177(8) 1 d D U . A -3
H3AA H 0.773822 0.483153 0.542205 0.135 Uiso 0.177(8) 1 calc R . . A -3
H3AB H 0.637802 0.442629 0.535494 0.135 Uiso 0.177(8) 1 calc R . . A -3
C4A C 0.715(2) 0.5503(19) 0.6003(10) 0.124(4) Uani 0.177(8) 1 d D U . A -3
H4AA H 0.798808 0.595451 0.612584 0.148 Uiso 0.177(8) 1 calc R . . A -3
H4AB H 0.665447 0.517224 0.634744 0.148 Uiso 0.177(8) 1 calc R . . A -3
C5A C 0.682(4) 0.637(3) 0.570(2) 0.137(4) Uani 0.177(8) 1 d D . . A -3
H5AA H 0.683399 0.628049 0.529005 0.205 Uiso 0.177(8) 1 calc GR . . A -3
H5AB H 0.738501 0.718327 0.581214 0.205 Uiso 0.177(8) 1 calc GR . . A -3
H5AC H 0.601797 0.617518 0.582095 0.205 Uiso 0.177(8) 1 calc GR . . A -3
N3B N 0.696(3) 0.641(3) 0.4429(18) 0.113(10) Uani 0.15 1 d . . . B 2
N3A N 0.6857(7) 0.666667 0.416667 0.117(7) Uani 0.7 2 d S T P B 1
C2 C 0.666667 0.333333 0.5093(7) 0.128(4) Uani 0.5 3 d S T P A 1
H2 H 0.576(8) 0.308(7) 0.508(3) 0.153 Uiso 0.5 1 d R . . C 1


_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 N2 2.2116(17) 31_655 ?
Mn1 N2 2.2115(17) . ?
Mn1 N2 2.2115(17) 2_655 ?
Mn1 N2 2.2115(17) 3_665 ?
Mn1 N2 2.2115(17) 32 ?
Mn1 N2 2.2115(17) 33_545 ?
N2 C1 1.109(2) . ?
C1 N3B 1.28(4) . ?
C1 N3B 1.44(4) 11_565 ?
C1 N3A 1.308(5) . ?
N1 C3 1.516(11) . ?
N1 C3A 1.447(19) . ?
N1 C2 1.705(17) . ?
N1 C2 1.705(17) 16_545 ?
C4 C3 1.428(10) . ?
C4 C5 1.534(11) . ?
C3A C4A 1.424(12) . ?
C4A C5A 1.530(13) . ?
N3B N3B 1.34(8) 11_565 ?

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
N2 Mn1 N2 88.60(8) 31_655 3_665 ?
N2 Mn1 N2 180.0 32 2_655 ?
N2 Mn1 N2 88.60(8) 32 . ?
N2 Mn1 N2 91.40(8) 31_655 32 ?
N2 Mn1 N2 180.0 31_655 . ?
N2 Mn1 N2 88.60(8) 3_665 32 ?
N2 Mn1 N2 91.40(8) 2_655 . ?
N2 Mn1 N2 91.40(8) 31_655 33_545 ?
N2 Mn1 N2 88.60(8) 33_545 2_655 ?
N2 Mn1 N2 180.0 3_665 33_545 ?
N2 Mn1 N2 91.40(8) 3_665 . ?
N2 Mn1 N2 91.40(8) 32 33_545 ?
N2 Mn1 N2 88.60(8) 33_545 . ?
N2 Mn1 N2 88.60(8) 31_655 2_655 ?
N2 Mn1 N2 91.40(8) 3_665 2_655 ?
C1 N2 Mn1 162.9(2) . . ?
N2 C1 N3B 150.2(17) . . ?
N2 C1 N3B 150.7(16) . 11_565 ?
N2 C1 N3A 170.7(4) . . ?
N3B C1 N3B 59(3) . 11_565 ?
N3A C1 N3B 30.6(15) . 11_565 ?
C3 N1 C2 72.4(5) . 16_545 ?
C3A N1 C2 108.2(9) . 16_545 ?
C2 N1 C2 180.0 . 16_545 ?
C3 C4 C5 110.8(11) . . ?
C4 C3 N1 123.2(11) . . ?
C4A C3A N1 125(2) . . ?
C3A C4A C5A 112.8(18) . . ?
C1 N3B C1 112(3) . 11_565 ?
C1 N3B N3B 67(3) . 11_565 ?
C1 N3A C1 119.4(7) 11_565 . ?

_olex2_exptl_crystal_mounting_method 
'piece of suitable crystal mounted on microloop sample holder and transferred to the driffractometer'
_olex2_submission_original_sample_id BurSt128
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_burst48_300k_0ma_a
_database_code_depnum_ccdc_archive 'CCDC 2068842'
loop_
_audit_author_name
_audit_author_address
'Stefan Burger'
;Technical University of Munich
Germany
;
_audit_update_record             
;
2021-03-08 deposited with the CCDC.	2021-06-14 downloaded from the CCDC.
;
_audit_creation_date             2021-03-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        C16H24N10Co
_chemical_formula_moiety         '0.25(C24 Co4 N36), 0.5(C20 H48 N2)'
_chemical_formula_sum            'C16 H24 Co N10'
_chemical_formula_weight         415.38
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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'

_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      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   10.0138(2)
_cell_length_b                   16.2151(4)
_cell_length_c                   12.7967(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2077.86(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    298
_cell_measurement_theta_max      26.367
_cell_measurement_theta_min      2.027
_shelx_estimated_absorpt_T_max   0.831
_shelx_estimated_absorpt_T_min   0.737
_exptl_absorpt_coefficient_mu    0.848
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.7031
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0693 before and 0.0450 after correction. The Ratio of minimum to maximum transmission is 0.9433. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear pinkish pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   pinkish
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             868
_exptl_crystal_preparation       
'suitable crystal selected and prepared under a microscope in perfluoro ether oil'
_exptl_crystal_recrystallization_method 
'mild solution approach from water at room temperature'
_exptl_crystal_size_max          0.384
_exptl_crystal_size_mid          0.305
_exptl_crystal_size_min          0.226
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_unetI/netI     0.0079
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            100185
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_min         2.027
_diffrn_ambient_temperature      297.99
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  IMS_Mo
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          none
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2049
_reflns_number_total             2206
_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       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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         0.247
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.034
_refine_ls_extinction_coef       0.0029(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         2206
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0252
_refine_ls_restrained_S_all      1.071
_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)+(0.0406P)²+0.5844P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0758
_refine_ls_wR_factor_ref         0.0780
_refine_special_details          none
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C7) = Uanis(C7A)
3. Others
 Fixed Sof: N3B(0.5) N6B(0.25) H4A(0.5) H4B(0.5) H4C(0.5) C5(0.5) H5A(0.5)
 H5B(0.5) C2(0.5) H2A(0.5) H2B(0.5) C3(0.5) H3A(0.5) H3B(0.5) C6(0.5) H6A(0.5)
 H6B(0.5) C6A(0.5) H6AA(0.5) H6AB(0.5) C1(0.5) H1A(0.5) H1B(0.5) H1C(0.5)
 C5A(0.5) H5AA(0.5) H5AB(0.5) C7A(0.5) H7AA(0.5) H7AB(0.5) H7AC(0.5) C7(0.5)
 H7A(0.5) H7B(0.5) H7C(0.5) N3A(0.5) N6A(0.25)
4.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C2(H2A,H2B), C3(H3A,H3B), C6(H6A,H6B), C6A(H6AA,H6AB), C5A(H5AA,
 H5AB)
4.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C1(H1A,H1B,H1C), C7A(H7AA,H7AB,H7AC), C7(H7A,H7B,H7C)
;
_atom_sites_solution_hydrogens   geom
_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
Co1 Co 1.000000 0.500000 0.500000 0.03321(12) Uani 1 2 d S T P . .
N1 N 0.60588(18) 0.250000 0.49798(12) 0.0470(4) Uani 1 2 d S T P . .
N5 N 1.03696(14) 0.38342(7) 0.43151(10) 0.0508(3) Uani 1 1 d . . . . .
N2 N 0.81850(14) 0.51336(9) 0.41696(10) 0.0587(4) Uani 1 1 d . . . . .
N4 N 0.60075(14) 0.55582(8) 0.12701(9) 0.0547(3) Uani 1 1 d . . . . .
N3B N 0.665(2) 0.5891(11) 0.3046(16) 0.064(3) Uani 0.5 1 d . . . A 2
C9 C 0.63095(14) 0.56571(9) 0.21165(11) 0.0456(3) Uani 1 1 d . . . . .
N6B N 1.1215(17) 0.250000 0.3725(12) 0.063(4) Uani 0.5 2 d S T P B 2
C10 C 1.06628(14) 0.31938(8) 0.40331(10) 0.0431(3) Uani 1 1 d . . . . .
C8 C 0.74425(14) 0.54378(10) 0.36192(10) 0.0470(3) Uani 1 1 d . . . . .
C4 C 0.5881(4) 0.250000 0.8009(2) 0.0797(8) Uani 1 2 d S T P . .
H4A H 0.497922 0.269753 0.796709 0.120 Uiso 0.5 1 calc GR . . C -1
H4B H 0.645723 0.294048 0.822844 0.120 Uiso 0.5 1 calc GR . . C -1
H4C H 0.592905 0.205694 0.850508 0.120 Uiso 0.5 1 calc GR . . C -1
C5 C 0.5737(3) 0.3215(2) 0.4263(3) 0.0540(7) Uani 0.5 1 d . . . D 1
H5A H 0.631108 0.367417 0.444619 0.065 Uiso 0.5 1 calc R . . D 1
H5B H 0.595336 0.305433 0.355251 0.065 Uiso 0.5 1 calc R . . D 1
C2 C 0.5880(3) 0.22104(19) 0.6114(2) 0.0552(7) Uani 0.5 1 d . . . D -1
H2A H 0.500680 0.243950 0.626572 0.066 Uiso 0.5 1 calc R . . D -1
H2B H 0.571185 0.162807 0.600094 0.066 Uiso 0.5 1 calc R . . D -1
C3 C 0.6324(3) 0.2190(2) 0.6938(3) 0.0630(8) Uani 0.5 1 d . . . D -1
H3A H 0.720138 0.243433 0.684955 0.076 Uiso 0.5 1 calc R . . D -1
H3B H 0.648695 0.160744 0.705272 0.076 Uiso 0.5 1 calc R . . D -1
C6 C 0.4317(4) 0.3505(3) 0.4287(3) 0.0671(9) Uani 0.5 1 d . . . D 1
H6A H 0.409841 0.368042 0.499150 0.081 Uiso 0.5 1 calc R . . D 1
H6B H 0.373446 0.304838 0.410968 0.081 Uiso 0.5 1 calc R . . D 1
C6A C 0.5132(4) 0.3569(3) 0.3689(3) 0.0701(10) Uani 0.5 1 d . . . D 2
H6AA H 0.601288 0.376663 0.349703 0.084 Uiso 0.5 1 calc R . . D 2
H6AB H 0.489735 0.312458 0.321668 0.084 Uiso 0.5 1 calc R . . D 2
C1 C 0.7497(3) 0.2263(2) 0.4799(3) 0.0701(13) Uani 0.5 1 d . . . D -1
H1A H 0.763965 0.216764 0.406709 0.105 Uiso 0.5 1 calc GR . . D -1
H1B H 0.769710 0.176985 0.518274 0.105 Uiso 0.5 1 calc GR . . D -1
H1C H 0.806834 0.270149 0.503179 0.105 Uiso 0.5 1 calc GR . . D -1
C5A C 0.5171(4) 0.3245(2) 0.4787(3) 0.0526(8) Uani 0.5 1 d . . . D 2
H5AA H 0.426706 0.310220 0.499122 0.063 Uiso 0.5 1 calc R . . D 2
H5AB H 0.546502 0.368723 0.524274 0.063 Uiso 0.5 1 calc R . . D 2
C7A C 0.416(4) 0.425(2) 0.357(3) 0.1007(17) Uani 0.5 1 d . . . D 2
H7AA H 0.429179 0.451095 0.290717 0.151 Uiso 0.5 1 calc GR . . D 2
H7AB H 0.428469 0.464008 0.412124 0.151 Uiso 0.5 1 calc GR . . D 2
H7AC H 0.326994 0.402732 0.360418 0.151 Uiso 0.5 1 calc GR . . D 2
C7 C 0.406(4) 0.421(2) 0.355(3) 0.1007(17) Uani 0.5 1 d . . . D 1
H7A H 0.403548 0.400083 0.284323 0.151 Uiso 0.5 1 calc GR . . D 1
H7B H 0.475373 0.460886 0.361218 0.151 Uiso 0.5 1 calc GR . . D 1
H7C H 0.321321 0.445580 0.371178 0.151 Uiso 0.5 1 calc GR . . D 1
N3A N 0.646(2) 0.5784(12) 0.3125(17) 0.066(3) Uani 0.5 1 d . . . A 1
N6A N 1.0890(16) 0.250000 0.3551(10) 0.061(4) Uani 0.5 2 d S T P B 1


_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 N5 2.1162(12) 5_766 ?
Co1 N5 2.1163(12) . ?
Co1 N2 2.1165(13) 5_766 ?
Co1 N2 2.1165(13) . ?
Co1 N4 2.1163(12) 2_665 ?
Co1 N4 2.1163(12) 6_656 ?
N1 C5 1.513(3) . ?
N1 C5 1.513(3) 7_565 ?
N1 C2 1.536(3) . ?
N1 C1 1.508(3) . ?
N1 C5A 1.521(4) 7_565 ?
N1 C5A 1.520(4) . ?
N5 C10 1.1378(17) . ?
N2 C8 1.1367(19) . ?
N4 C9 1.1359(17) . ?
N3B C9 1.29(2) . ?
N3B C8 1.31(2) . ?
C9 N3A 1.32(2) . ?
N6B C10 1.314(8) 7_565 ?
N6B C10 1.314(8) . ?
C10 N6A 1.303(7) . ?
C8 N3A 1.29(2) . ?
C4 C3 1.526(4) . ?
C5 C6 1.498(5) . ?
C2 C3 1.144(4) . ?
C6 C7 1.50(4) . ?
C6A C5A 1.501(5) . ?
C6A C7A 1.47(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N5 Co1 N5 180.0 5_766 . ?
N5 Co1 N2 91.93(5) . . ?
N5 Co1 N2 91.93(5) 5_766 5_766 ?
N5 Co1 N2 88.07(5) . 5_766 ?
N5 Co1 N2 88.07(5) 5_766 . ?
N5 Co1 N4 91.11(5) 5_766 6_656 ?
N5 Co1 N4 88.89(5) 5_766 2_665 ?
N2 Co1 N2 180.0 . 5_766 ?
N4 Co1 N5 88.89(5) 6_656 . ?
N4 Co1 N5 91.11(5) 2_665 . ?
N4 Co1 N2 88.86(5) 2_665 5_766 ?
N4 Co1 N2 91.14(6) 2_665 . ?
N4 Co1 N2 88.86(5) 6_656 . ?
N4 Co1 N2 91.14(6) 6_656 5_766 ?
N4 Co1 N4 180.00(6) 6_656 2_665 ?
C5 N1 C5 100.0(3) 7_565 . ?
C5 N1 C2 108.31(18) 7_565 . ?
C5 N1 C2 141.5(2) . . ?
C5 N1 C5A 112.7(2) . 7_565 ?
C5 N1 C5A 33.71(16) 7_565 7_565 ?
C1 N1 C5 85.1(2) . 7_565 ?
C1 N1 C5 107.8(2) . . ?
C1 N1 C2 100.3(2) . . ?
C1 N1 C5A 109.3(2) . 7_565 ?
C5A N1 C5A 105.3(3) . 7_565 ?
C10 N5 Co1 172.59(13) . . ?
C8 N2 Co1 156.52(14) . . ?
C9 N4 Co1 156.86(13) . 2_664 ?
C9 N3B C8 120.6(12) . . ?
N4 C9 N3B 171.0(9) . . ?
N4 C9 N3A 171.3(9) . . ?
C10 N6B C10 117.7(12) . 7_565 ?
N5 C10 N6B 170.1(7) . . ?
N5 C10 N6A 169.4(6) . . ?
N2 C8 N3B 171.5(8) . . ?
N2 C8 N3A 170.4(9) . . ?
C6 C5 N1 115.5(3) . . ?
C3 C2 N1 146.5(3) . . ?
C2 C3 C4 134.8(3) . . ?
C5 C6 C7 112.9(14) . . ?
C7A C6A C5A 112.0(14) . . ?
C6A C5A N1 116.5(3) . . ?
C8 N3A C9 120.0(13) . . ?
C10 N6A C10 119.4(10) . 7_565 ?

_olex2_exptl_crystal_mounting_method 
'suitable piece of crystal was mounted on top of a MiGeTen sample holder'
_olex2_submission_original_sample_id BurSt48
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_burst19_298k_1_0ma_a
_database_code_depnum_ccdc_archive 'CCDC 2068843'
loop_
_audit_author_name
_audit_author_address
'Stefan Burger'
;Technical University of Munich
Germany
;
_audit_update_record             
;
2021-03-08 deposited with the CCDC.	2021-06-14 downloaded from the CCDC.
;
_audit_creation_date             2021-03-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        C16H24N10Mn
_chemical_formula_moiety         '0.25(C24 Mn4 N36), C10 H24 N'
_chemical_formula_sum            'C16 H24 Mn N10'
_chemical_formula_weight         411.39
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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'

_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      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   10.0193(5)
_cell_length_b                   16.4215(10)
_cell_length_c                   13.0125(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2141.0(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7289
_cell_measurement_temperature    298
_cell_measurement_theta_max      26.371
_cell_measurement_theta_min      1.997
_shelx_estimated_absorpt_T_max   0.847
_shelx_estimated_absorpt_T_min   0.839
_exptl_absorpt_coefficient_mu    0.638
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6510
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0527 before and 0.0452 after correction. The Ratio of minimum to maximum transmission is 0.8721. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             860
_exptl_crystal_preparation       
'suitable crystal was selected and cut under a microscope'
_exptl_crystal_recrystallization_method 
'mild solution approach from water at room temperature'
_exptl_crystal_size_max          0.285
_exptl_crystal_size_mid          0.278
_exptl_crystal_size_min          0.27
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            28206
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         1.997
_diffrn_ambient_temperature      298.04
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  D8_Triumph
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          none
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1664
_reflns_number_total             2271
_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       'SAINT V8.40A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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         0.211
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.032
_refine_ls_extinction_coef       0.0424(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         2271
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0294
_refine_ls_restrained_S_all      1.020
_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)+(0.0405P)²+0.6049P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0888
_refine_special_details          none
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Others
 Fixed Sof: N6B(0.25) H4A(0.5) H4B(0.5) H4C(0.5) C5(0.5) H5A(0.5) H5B(0.5)
 C2(0.5) H2A(0.5) H2B(0.5) C7(0.5) H7A(0.5) H7B(0.5) C8(0.5) H8A(0.5) H8B(0.5)
 C6(0.5) H6A(0.5) H6B(0.5) C3(0.5) H3A(0.5) H3B(0.5) C1(0.5) H1A(0.5) H1B(0.5)
 H1C(0.5) H9AA(0.5) H9AB(0.5) H9AC(0.5) H9BD(0.5) H9BE(0.5) H9BF(0.5) N6A(0.25)
3.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C2(H2A,H2B), C7(H7A,H7B), C8(H8A,H8B), C6(H6A,H6B), C3(H3A,H3B)
3.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C1(H1A,H1B,H1C), C9(H9AA,H9AB,H9AC), C9(H9BD,H9BE,H9BF)
;
_atom_sites_solution_hydrogens   geom
_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 0.500000 0.500000 1.000000 0.04273(16) Uani 1 2 d S T P . .
N1 N 0.3938(2) 0.750000 0.49686(15) 0.0563(6) Uani 1 2 d S T P . .
N5 N 0.54211(19) 0.38158(10) 0.92576(13) 0.0685(5) Uani 1 1 d . . . . .
N4 N 0.8096(2) 0.51257(12) 0.58506(14) 0.0797(6) Uani 1 1 d . . . . .
N2 N 0.60418(19) 0.56218(11) 0.87241(13) 0.0739(5) Uani 1 1 d . . . . .
N3 N 0.65247(19) 0.58617(12) 0.69194(12) 0.0814(6) Uani 1 1 d . . . . .
C11 C 0.63116(18) 0.56997(11) 0.78819(15) 0.0570(5) Uani 1 1 d . . . . .
N6B N 0.5932(19) 0.250000 0.8521(10) 0.077(5) Uani 0.5 2 d S T P A 2
C13 C 0.57126(18) 0.31848(11) 0.89856(13) 0.0543(4) Uani 1 1 d . . . . .
C12 C 0.73821(19) 0.54450(13) 0.63947(14) 0.0598(5) Uani 1 1 d . . . . .
C4 C 0.4097(4) 0.750000 0.7949(2) 0.0893(10) Uani 1 2 d S T P . .
H4A H 0.501366 0.766954 0.792195 0.134 Uiso 0.5 1 calc GR . . B -1
H4B H 0.400234 0.706781 0.844003 0.134 Uiso 0.5 1 calc GR . . B -1
H4C H 0.354861 0.795199 0.814967 0.134 Uiso 0.5 1 calc GR . . B -1
C5 C 0.4251(5) 0.6787(3) 0.4273(5) 0.0651(11) Uani 0.5 1 d . . . C 1
H5A H 0.367148 0.633802 0.445890 0.078 Uiso 0.5 1 calc R . . C 1
H5B H 0.403592 0.694125 0.357234 0.078 Uiso 0.5 1 calc R . . C 1
C2 C 0.4113(4) 0.7215(2) 0.6090(3) 0.0658(11) Uani 0.5 1 d . . . C -1
H2A H 0.426793 0.663790 0.598142 0.079 Uiso 0.5 1 calc R . . C -1
H2B H 0.499062 0.743406 0.623764 0.079 Uiso 0.5 1 calc R . . C -1
C7 C 0.5661(5) 0.6493(3) 0.4297(4) 0.0793(13) Uani 0.5 1 d . . . C 1
H7A H 0.589028 0.632865 0.499104 0.095 Uiso 0.5 1 calc R . . C 1
H7B H 0.625495 0.693197 0.409816 0.095 Uiso 0.5 1 calc R . . C 1
C8 C 0.4844(6) 0.6436(3) 0.3700(4) 0.0851(14) Uani 0.5 1 d . . . C 2
H8A H 0.396834 0.622548 0.352695 0.102 Uiso 0.5 1 calc R . . C 2
H8B H 0.504700 0.687604 0.322793 0.102 Uiso 0.5 1 calc R . . C 2
C6 C 0.4820(6) 0.6762(3) 0.4776(4) 0.0650(12) Uani 0.5 1 d . . . C 2
H6A H 0.572624 0.690209 0.496869 0.078 Uiso 0.5 1 calc R . . C 2
H6B H 0.452984 0.632762 0.522944 0.078 Uiso 0.5 1 calc R . . C 2
C3 C 0.3668(4) 0.7201(3) 0.6899(3) 0.0757(13) Uani 0.5 1 d . . . C -1
H3A H 0.348956 0.662779 0.701216 0.091 Uiso 0.5 1 calc R . . C -1
H3B H 0.279731 0.745003 0.680776 0.091 Uiso 0.5 1 calc R . . C -1
C1 C 0.2490(4) 0.7279(3) 0.4792(4) 0.083(2) Uani 0.5 1 d . . . C -1
H1A H 0.233675 0.720223 0.407066 0.125 Uiso 0.5 1 calc GR . . C -1
H1B H 0.192938 0.770983 0.504157 0.125 Uiso 0.5 1 calc GR . . C -1
H1C H 0.228590 0.678452 0.515324 0.125 Uiso 0.5 1 calc GR . . C -1
C9 C 0.5851(3) 0.57788(18) 0.3574(2) 0.1101(10) Uani 1 1 d . . . . .
H9AA H 0.516834 0.538036 0.369933 0.165 Uiso 0.5 1 calc GR . . C 1
H9AB H 0.671127 0.553869 0.368965 0.165 Uiso 0.5 1 calc GR . . C 1
H9AC H 0.579190 0.596471 0.287648 0.165 Uiso 0.5 1 calc GR . . C 1
H9BD H 0.579844 0.541197 0.414753 0.165 Uiso 0.5 1 calc GR . . C 2
H9BE H 0.672713 0.601358 0.354449 0.165 Uiso 0.5 1 calc GR . . C 2
H9BF H 0.567607 0.548606 0.295012 0.165 Uiso 0.5 1 calc GR . . C 2
N6A N 0.6261(19) 0.250000 0.8689(13) 0.085(5) Uani 0.5 2 d S T P A 1


_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 N5 2.2120(16) . ?
Mn1 N5 2.2120(16) 5_667 ?
Mn1 N4 2.2151(19) 2_665 ?
Mn1 N4 2.2151(19) 6_557 ?
Mn1 N2 2.2110(16) . ?
Mn1 N2 2.2111(16) 5_667 ?
N1 C5 1.513(5) 7_575 ?
N1 C5 1.513(5) . ?
N1 C2 1.542(4) . ?
N1 C6 1.521(5) . ?
N1 C6 1.521(5) 7_575 ?
N1 C1 1.513(4) . ?
N5 C13 1.133(2) . ?
N4 C12 1.135(2) . ?
N2 C11 1.136(2) . ?
N3 C11 1.298(2) . ?
N3 C12 1.293(3) . ?
N6B C13 1.295(6) . ?
N6B C13 1.295(6) 7_565 ?
C13 N6A 1.310(9) . ?
C4 C3 1.514(5) . ?
C5 C7 1.494(6) . ?
C2 C3 1.144(5) . ?
C7 C9 1.515(6) . ?
C8 C6 1.498(7) . ?
C8 C9 1.486(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N5 Mn1 N5 180.00(8) . 5_667 ?
N5 Mn1 N4 91.60(7) 5_667 2_665 ?
N5 Mn1 N4 91.60(7) . 6_557 ?
N5 Mn1 N4 88.40(7) 5_667 6_557 ?
N5 Mn1 N4 88.40(7) . 2_665 ?
N4 Mn1 N4 180.0 2_665 6_557 ?
N2 Mn1 N5 89.31(6) . . ?
N2 Mn1 N5 89.31(6) 5_667 5_667 ?
N2 Mn1 N5 90.69(6) 5_667 . ?
N2 Mn1 N5 90.69(6) . 5_667 ?
N2 Mn1 N4 90.67(7) . 2_665 ?
N2 Mn1 N4 89.33(7) . 6_557 ?
N2 Mn1 N4 89.33(7) 5_667 2_665 ?
N2 Mn1 N4 90.67(7) 5_667 6_557 ?
N2 Mn1 N2 180.0 . 5_667 ?
C5 N1 C5 101.4(4) 7_575 . ?
C5 N1 C2 107.9(3) . . ?
C5 N1 C2 141.1(3) 7_575 . ?
C5 N1 C6 113.4(3) . 7_575 ?
C5 N1 C6 33.28(19) 7_575 7_575 ?
C5 N1 C1 107.1(3) 7_575 . ?
C5 N1 C1 85.6(3) . . ?
C6 N1 C6 105.7(4) 7_575 . ?
C1 N1 C2 100.3(3) . . ?
C1 N1 C6 136.3(3) . 7_575 ?
C13 N5 Mn1 171.65(17) . . ?
C12 N4 Mn1 153.84(19) . 2_664 ?
C11 N2 Mn1 152.72(18) . . ?
C12 N3 C11 120.68(17) . . ?
N2 C11 N3 173.2(2) . . ?
C13 N6B C13 120.5(10) . 7_565 ?
N5 C13 N6B 169.5(7) . . ?
N5 C13 N6A 170.1(8) . . ?
N4 C12 N3 173.0(2) . . ?
C7 C5 N1 115.7(5) . . ?
C3 C2 N1 146.4(4) . . ?
C5 C7 C9 110.9(4) . . ?
C9 C8 C6 111.9(4) . . ?
C8 C6 N1 116.6(5) . . ?
C2 C3 C4 135.5(4) . . ?
C13 N6A C13 118.3(13) . 7_565 ?

_olex2_exptl_crystal_mounting_method 
'after selecting suitable crystal in perfluoroether oil, it was mounted on top of a MiTeGen sample holder'
_olex2_submission_original_sample_id BurSt19
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_mo_burst129_100k_0m_b
_database_code_depnum_ccdc_archive 'CCDC 2068848'
loop_
_audit_author_name
_audit_author_address
'Stefan Burger'
;Technical University of Munich
Germany
;
_audit_update_record             
;
2021-03-08 deposited with the CCDC.	2021-06-14 downloaded from the CCDC.
;
_audit_creation_date             2021-03-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        C16H24N10Mn
_chemical_formula_moiety         '0.17(C36 Mn6 N54), 1(C10 H24 N1)'
_chemical_formula_sum            'C16 H24 Mn N10'
_chemical_formula_weight         411.39
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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'

_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      trigonal
_space_group_IT_number           161
_space_group_name_H-M_alt        'R 3 c'
_space_group_name_Hall           'R 3 -2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'

_cell_length_a                   12.8301(13)
_cell_length_b                   12.8301(13)
_cell_length_c                   21.750(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3100.7(8)
_cell_formula_units_Z            5.99994
_cell_measurement_reflns_used    8007
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.864
_cell_measurement_theta_min      2.058
_shelx_estimated_absorpt_T_max   0.933
_shelx_estimated_absorpt_T_min   0.893
_exptl_absorpt_coefficient_mu    0.661
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5641
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0939 before and 0.0805 after correction. The Ratio of minimum to maximum transmission is 0.7565. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1290
_exptl_crystal_preparation       
'suitable crystal prepared from bulk in perfluoroether oil under a microscope'
_exptl_crystal_recrystallization_method 
'high entropy crystallisation from water precursor solution at 95 degrees C'
_exptl_crystal_size_max          0.176
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.107
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0675
_diffrn_reflns_av_unetI/netI     0.0377
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            14822
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.864
_diffrn_reflns_theta_min         2.621
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  TXS
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          none
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.990
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                1477
_reflns_number_total             1650
_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       'SAINT V8.40A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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         0.857
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.36(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     87
_refine_ls_number_reflns         1650
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0396
_refine_ls_restrained_S_all      1.082
_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)+(0.0515P)²+6.5785P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0983
_refine_ls_wR_factor_ref         0.1039
_refine_special_details          none,Twin
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.64(5)
 0.36(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B)
3.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C)
;
_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 0.333333 0.666667 0.64252(6) 0.0161(2) Uani 1 3 d S T P . .
N1 N 0.666667 0.333333 0.5485(3) 0.0200(16) Uani 1 3 d S T P . .
N4 N 0.8553(4) 0.8546(3) 0.53183(19) 0.0280(9) Uani 1 1 d . . . . .
N3 N 0.6496(3) 0.6832(3) 0.52921(19) 0.0314(9) Uani 1 1 d . . . . .
N2 N 0.4762(3) 0.6743(4) 0.5829(2) 0.0251(8) Uani 1 1 d . . . . .
C2 C 0.7565(4) 0.7775(4) 0.5317(2) 0.0236(8) Uani 1 1 d . . . . .
C1 C 0.5608(4) 0.6842(4) 0.5589(2) 0.0223(8) Uani 1 1 d . . . . .
C4 C 0.5832(4) 0.3765(4) 0.5248(2) 0.0245(9) Uani 1 1 d . . . . .
H4A H 0.607523 0.455725 0.543580 0.029 Uiso 1 1 calc R . . . .
H4B H 0.594824 0.388823 0.479800 0.029 Uiso 1 1 calc R . . . .
C5 C 0.4501(4) 0.2932(4) 0.5372(2) 0.0281(9) Uani 1 1 d . . . . .
H5A H 0.438659 0.264702 0.580290 0.034 Uiso 1 1 calc R . . . .
H5B H 0.418900 0.222195 0.509864 0.034 Uiso 1 1 calc R . . . .
C3 C 0.666667 0.333333 0.6180(4) 0.0291(17) Uani 1 3 d S T P . .
C6 C 0.3802(4) 0.3589(4) 0.5261(2) 0.0308(10) Uani 1 1 d . . . . .
H6A H 0.401065 0.397415 0.485593 0.046 Uiso 1 1 calc GR . . . .
H6B H 0.401001 0.420286 0.557920 0.046 Uiso 1 1 calc GR . . . .
H6C H 0.293668 0.301111 0.527688 0.046 Uiso 1 1 calc GR . . . .
H3 H 0.585(6) 0.269(5) 0.631(3) 0.046 Uiso 1 1 d R . . . .


_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 N4 2.224(4) 18_454 ?
Mn1 N4 2.224(4) 16_664 ?
Mn1 N4 2.224(4) 17_544 ?
Mn1 N2 2.208(4) 2_665 ?
Mn1 N2 2.208(4) 3_565 ?
Mn1 N2 2.208(4) . ?
N1 C4 1.521(5) 3_665 ?
N1 C4 1.521(5) . ?
N1 C4 1.521(5) 2_655 ?
N1 C3 1.511(9) . ?
N4 C2 1.153(6) . ?
N3 C2 1.300(6) . ?
N3 C1 1.315(6) . ?
N2 C1 1.152(6) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C5 1.519(6) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.525(6) . ?
C3 H3 1.00(7) . ?
C3 H3 1.00(6) 2_655 ?
C3 H3 1.00(6) 3_665 ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?

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
N4 Mn1 N4 92.89(16) 16_664 17_544 ?
N4 Mn1 N4 92.89(16) 18_454 16_664 ?
N4 Mn1 N4 92.89(16) 18_454 17_544 ?
N2 Mn1 N4 90.79(15) 2_665 16_664 ?
N2 Mn1 N4 176.29(18) 2_665 17_544 ?
N2 Mn1 N4 90.79(15) 3_565 18_454 ?
N2 Mn1 N4 90.79(15) . 17_544 ?
N2 Mn1 N4 176.29(18) . 18_454 ?
N2 Mn1 N4 87.33(15) 2_665 18_454 ?
N2 Mn1 N4 176.29(18) 3_565 16_664 ?
N2 Mn1 N4 87.32(15) . 16_664 ?
N2 Mn1 N4 87.33(15) 3_565 17_544 ?
N2 Mn1 N2 88.97(17) 3_565 . ?
N2 Mn1 N2 88.97(17) 2_665 3_565 ?
N2 Mn1 N2 88.97(17) 2_665 . ?
C4 N1 C4 109.1(3) 2_655 . ?
C4 N1 C4 109.1(3) 3_665 . ?
C4 N1 C4 109.1(3) 2_655 3_665 ?
C3 N1 C4 109.8(3) . . ?
C3 N1 C4 109.8(3) . 2_655 ?
C3 N1 C4 109.8(3) . 3_665 ?
C2 N4 Mn1 144.7(4) . 10_664 ?
C2 N3 C1 119.1(4) . . ?
C1 N2 Mn1 170.5(4) . . ?
N4 C2 N3 173.7(5) . . ?
N2 C1 N3 173.6(4) . . ?
N1 C4 H4A 108.4 . . ?
N1 C4 H4B 108.4 . . ?
H4A C4 H4B 107.4 . . ?
C5 C4 N1 115.6(3) . . ?
C5 C4 H4A 108.4 . . ?
C5 C4 H4B 108.4 . . ?
C4 C5 H5A 109.6 . . ?
C4 C5 H5B 109.6 . . ?
C4 C5 C6 110.4(4) . . ?
H5A C5 H5B 108.1 . . ?
C6 C5 H5A 109.6 . . ?
C6 C5 H5B 109.6 . . ?
N1 C3 H3 107(4) . 3_665 ?
N1 C3 H3 107(4) . . ?
N1 C3 H3 107(4) . 2_655 ?
H3 C3 H3 112(4) 2_655 3_665 ?
H3 C3 H3 112(4) . 2_655 ?
H3 C3 H3 112(4) . 3_665 ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?

_olex2_exptl_crystal_mounting_method 
'suitable crystal was mounted on top of a microloop sample holder and transferred to the diffractometer'
_olex2_submission_original_sample_id BurSt129
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.64(5)
2 0.36(5)

####################################################################### 
# 
# 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_burst39_0ma_a
_database_code_depnum_ccdc_archive 'CCDC 2068716'
loop_
_audit_author_name
_audit_author_address
'Stefan Burger'
;Technical University of Munich
Germany
;
_audit_update_record             
;
2021-03-08 deposited with the CCDC.	2021-06-14 downloaded from the CCDC.
;
_audit_creation_date             2021-03-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        C16H24N10Ni
_chemical_formula_moiety         '0.25(C24 N36 Ni4), 0.5(C20 H48 N2)'
_chemical_formula_sum            'C16 H24 N10 Ni'
_chemical_formula_weight         415.16
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   10.0232(3)
_cell_length_b                   16.1193(5)
_cell_length_c                   12.6992(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2051.77(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9939
_cell_measurement_temperature    300
_cell_measurement_theta_max      28.699
_cell_measurement_theta_min      2.527
_shelx_estimated_absorpt_T_max   0.846
_shelx_estimated_absorpt_T_min   0.786
_exptl_absorpt_coefficient_mu    0.968
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6964
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0940 before and 0.0494 after correction. The Ratio of minimum to maximum transmission is 0.9336. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear greenish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             872
_exptl_crystal_preparation       
'suitable crystal was cut and prepared under a microscope in perfluoroether oil'
_exptl_crystal_recrystallization_method 
'mild solution approach in water at room temperature'
_exptl_crystal_size_max          0.261
_exptl_crystal_size_mid          0.219
_exptl_crystal_size_min          0.179
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_unetI/netI     0.0094
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            77417
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.699
_diffrn_reflns_theta_min         2.527
_diffrn_ambient_temperature      300.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  TXS
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          none
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2162
_reflns_number_total             2734
_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       'SAINT V8.40A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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         0.280
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       0.0090(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         2734
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0283
_refine_ls_restrained_S_all      1.051
_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)+(0.0372P)²+0.7808P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0738
_refine_ls_wR_factor_ref         0.0805
_refine_special_details          none
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C9) = Uanis(C4) = Uanis(C10)
3. Others
 Fixed Sof: N3A(0.5) N6A(0.25) H4A(0.5) H4B(0.5) H4C(0.5) C9(0.5) H9A(0.5)
 H9B(0.5) H9C(0.5) C6(0.5) H6A(0.5) H6B(0.5) C2(0.5) H2A(0.5) H2B(0.5) C3(0.5)
 H3A(0.5) H3B(0.5) C7(0.5) H7A(0.5) H7B(0.5) C8(0.5) H8A(0.5) H8B(0.5) C5(0.5)
 H5A(0.5) H5B(0.5) C10(0.5) H10A(0.5) H10B(0.5) H10C(0.5) C1(0.5) H1A(0.5)
 H1B(0.5) H1C(0.5) N6(0.25) N3(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C2(H2A,H2B), C3(H3A,H3B), C7(H7A,H7B), C8(H8A,H8B), C5(H5A,H5B)
4.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_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
Ni1 Ni 1.000000 0.500000 0.500000 0.02816(10) Uani 1 2 d S T P . .
N1 N 0.39487(19) 0.750000 0.50158(13) 0.0418(4) Uani 1 2 d S T P . .
N5 N 1.03387(15) 0.38430(8) 0.43373(10) 0.0441(3) Uani 1 1 d . . . . .
N4 N 0.59925(14) 0.55377(8) 0.12625(10) 0.0469(3) Uani 1 1 d . . . . .
N2 N 0.82227(15) 0.51329(9) 0.41743(11) 0.0498(4) Uani 1 1 d . . . . .
N3A N 0.6482(18) 0.5745(11) 0.3131(14) 0.062(4) Uani 0.5 1 d . . . A 2
N6A N 1.0845(15) 0.250000 0.3568(11) 0.053(4) Uani 0.5 2 d S T P B 2
C12 C 0.63051(15) 0.56387(9) 0.21129(12) 0.0404(3) Uani 1 1 d . . . . .
C13 C 1.06329(15) 0.31996(9) 0.40522(11) 0.0384(3) Uani 1 1 d . . . . .
C11 C 0.74682(15) 0.54315(10) 0.36230(11) 0.0410(3) Uani 1 1 d . . . . .
C4 C 0.4120(3) 0.750000 0.1963(2) 0.0686(6) Uani 1 2 d S T P . .
H4A H 0.500452 0.727426 0.200941 0.103 Uiso 0.5 1 calc GR . . C -1
H4B H 0.411443 0.795210 0.147081 0.103 Uiso 0.5 1 calc GR . . C -1
H4C H 0.351498 0.707702 0.172827 0.103 Uiso 0.5 1 calc GR . . C -1
C9 C 0.6026(6) 0.5887(3) 0.6563(4) 0.0686(6) Uani 0.5 1 d . . . D 1
H9A H 0.678581 0.556375 0.635665 0.103 Uiso 0.5 1 calc GR . . D 1
H9B H 0.527532 0.552743 0.667357 0.103 Uiso 0.5 1 calc GR . . D 1
H9C H 0.622333 0.617825 0.720424 0.103 Uiso 0.5 1 calc GR . . D 1
C6 C 0.4274(4) 0.6783(2) 0.5739(3) 0.0484(8) Uani 0.5 1 d . . . D 1
H6A H 0.405193 0.694331 0.645408 0.058 Uiso 0.5 1 calc R . . D 1
H6B H 0.370679 0.631817 0.555218 0.058 Uiso 0.5 1 calc R . . D 1
C2 C 0.4121(4) 0.7791(2) 0.3872(3) 0.0503(8) Uani 0.5 1 d . . . D -1
H2A H 0.428603 0.837656 0.398660 0.060 Uiso 0.5 1 calc R . . D -1
H2B H 0.499558 0.756234 0.372001 0.060 Uiso 0.5 1 calc R . . D -1
C3 C 0.3686(4) 0.7812(2) 0.3043(3) 0.0579(9) Uani 0.5 1 d . . . D -1
H3A H 0.353284 0.839944 0.292733 0.070 Uiso 0.5 1 calc R . . D -1
H3B H 0.280526 0.757239 0.313033 0.070 Uiso 0.5 1 calc R . . D -1
C7 C 0.5703(4) 0.6497(3) 0.5718(3) 0.0641(10) Uani 0.5 1 d . . . D 1
H7A H 0.588638 0.624610 0.503876 0.077 Uiso 0.5 1 calc R . . D 1
H7B H 0.628203 0.697556 0.579211 0.077 Uiso 0.5 1 calc R . . D 1
C8 C 0.4871(5) 0.6423(3) 0.6310(3) 0.0655(11) Uani 0.5 1 d . . . D 2
H8A H 0.398145 0.626386 0.653259 0.079 Uiso 0.5 1 calc R . . D 2
H8B H 0.520137 0.684528 0.678745 0.079 Uiso 0.5 1 calc R . . D 2
C5 C 0.4837(4) 0.6751(2) 0.5205(3) 0.0482(8) Uani 0.5 1 d . . . D 2
H5A H 0.454472 0.630813 0.474239 0.058 Uiso 0.5 1 calc R . . D 2
H5B H 0.573985 0.689686 0.500123 0.058 Uiso 0.5 1 calc R . . D 2
C10 C 0.5809(6) 0.5659(3) 0.6321(4) 0.0686(6) Uani 0.5 1 d . . . D 2
H10A H 0.547672 0.524770 0.584176 0.103 Uiso 0.5 1 calc GR . . D 2
H10B H 0.584159 0.543172 0.701922 0.103 Uiso 0.5 1 calc GR . . D 2
H10C H 0.668841 0.582534 0.610952 0.103 Uiso 0.5 1 calc GR . . D 2
C1 C 0.2513(3) 0.7263(3) 0.5199(3) 0.0637(13) Uani 0.5 1 d . . . D -1
H1A H 0.236679 0.717621 0.593784 0.096 Uiso 0.5 1 calc GR . . D -1
H1B H 0.231502 0.676195 0.482171 0.096 Uiso 0.5 1 calc GR . . D -1
H1C H 0.194174 0.770064 0.495385 0.096 Uiso 0.5 1 calc GR . . D -1
N6 N 1.1192(16) 0.250000 0.3729(13) 0.054(4) Uani 0.5 2 d S T P B 1
N3 N 0.6635(19) 0.5893(11) 0.3051(14) 0.057(3) Uani 0.5 1 d . . . A 1


_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
Ni1 N5 2.0741(13) 5_766 ?
Ni1 N5 2.0741(13) . ?
Ni1 N4 2.0764(12) 2_665 ?
Ni1 N4 2.0764(12) 6_656 ?
Ni1 N2 2.0781(14) 5_766 ?
Ni1 N2 2.0782(14) . ?
N1 C6 1.511(4) 7_575 ?
N1 C6 1.511(4) . ?
N1 C2 1.536(4) . ?
N1 C5 1.518(4) 7_575 ?
N1 C5 1.518(4) . ?
N1 C1 1.507(4) . ?
N5 C13 1.1374(19) . ?
N4 C12 1.1362(18) . ?
N2 C11 1.1375(19) . ?
N3A C12 1.316(18) . ?
N3A C11 1.274(18) . ?
N6A C13 1.302(7) . ?
N6A C13 1.302(7) 7_565 ?
C12 N3 1.302(16) . ?
C13 N6 1.324(9) . ?
C11 N3 1.333(18) . ?
C4 C3 1.525(4) . ?
C9 C7 1.491(7) . ?
C6 C7 1.505(5) . ?
C2 C3 1.140(4) . ?
C8 C5 1.501(5) . ?
C8 C10 1.549(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N5 Ni1 N5 180.00(8) 5_766 . ?
N5 Ni1 N4 89.06(5) . 6_656 ?
N5 Ni1 N4 90.94(5) . 2_665 ?
N5 Ni1 N4 90.94(5) 5_766 6_656 ?
N5 Ni1 N4 89.06(5) 5_766 2_665 ?
N5 Ni1 N2 88.38(6) . 5_766 ?
N5 Ni1 N2 91.62(6) . . ?
N5 Ni1 N2 88.38(6) 5_766 . ?
N5 Ni1 N2 91.62(6) 5_766 5_766 ?
N4 Ni1 N4 180.00(7) 6_656 2_665 ?
N4 Ni1 N2 91.25(6) 6_656 5_766 ?
N4 Ni1 N2 91.25(6) 2_665 . ?
N4 Ni1 N2 88.75(6) 6_656 . ?
N4 Ni1 N2 88.75(6) 2_665 5_766 ?
N2 Ni1 N2 180.0 5_766 . ?
C6 N1 C6 99.7(3) 7_575 . ?
C6 N1 C2 108.5(2) 7_575 . ?
C6 N1 C2 141.6(2) . . ?
C6 N1 C5 112.7(2) . 7_575 ?
C6 N1 C5 33.93(17) 7_575 7_575 ?
C5 N1 C5 105.2(3) . 7_575 ?
C1 N1 C6 107.8(2) . 7_575 ?
C1 N1 C6 85.3(2) . . ?
C1 N1 C2 109.3(2) . . ?
C1 N1 C5 137.5(2) . 7_575 ?
C13 N5 Ni1 172.54(14) . . ?
C12 N4 Ni1 157.80(14) . 2_664 ?
C11 N2 Ni1 157.54(15) . . ?
C11 N3A C12 122.3(12) . . ?
C13 N6A C13 120.1(11) 7_565 . ?
N4 C12 N3A 171.7(8) . . ?
N4 C12 N3 169.9(8) . . ?
N5 C13 N6A 169.3(7) . . ?
N5 C13 N6 170.0(7) . . ?
N2 C11 N3A 170.3(9) . . ?
N2 C11 N3 171.0(7) . . ?
C7 C6 N1 115.4(3) . . ?
C3 C2 N1 147.1(4) . . ?
C2 C3 C4 135.3(4) . . ?
C9 C7 C6 113.3(4) . . ?
C5 C8 C10 107.6(4) . . ?
C8 C5 N1 116.2(3) . . ?
C13 N6 C13 116.8(12) 7_565 . ?
C12 N3 C11 118.8(12) . . ?

_olex2_exptl_crystal_mounting_method 
'suitable piece of crystal was mounted on top of a MiTeGen sample holder'
_olex2_submission_original_sample_id BurSt39
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_mo_burst120_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2068847'
loop_
_audit_author_name
_audit_author_address
'Stefan Burger'
;Technical University of Munich
Germany
;
_audit_update_record             
;
2021-03-08 deposited with the CCDC.	2021-06-14 downloaded from the CCDC.
;
_audit_creation_date             2021-03-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        C16H24CoN10
_chemical_formula_moiety         '0.17(C36 Co6 N54), 1(C9 H21 N1), 2(C0.5 H1.5)'
_chemical_formula_sum            'C16 H24 Co N10'
_chemical_formula_weight         415.37
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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'

_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      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c'
_space_group_name_Hall           '-R 3 2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   12.6131(2)
_cell_length_b                   12.6131(2)
_cell_length_c                   22.8639(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3150.10(13)
_cell_formula_units_Z            6.00012
_cell_measurement_reflns_used    9741
_cell_measurement_temperature    350(2)
_cell_measurement_theta_max      29.42
_cell_measurement_theta_min      2.58
_shelx_estimated_absorpt_T_max   0.890
_shelx_estimated_absorpt_T_min   0.838
_exptl_absorpt_coefficient_mu    0.839
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.7179
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0605 before and 0.0392 after correction.
The Ratio of minimum to maximum transmission is 0.9619.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear pinkish pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   pinkish
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1302
_exptl_crystal_preparation       
'suitable crystal was prepared in perfluoroether oil under a microscope'
_exptl_crystal_recrystallization_method 
'high entropy crystallisation from water precursor solution at 95 degree C'
_exptl_crystal_size_max          0.218
_exptl_crystal_size_mid          0.157
_exptl_crystal_size_min          0.142
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_unetI/netI     0.0084
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            17146
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.689
_diffrn_reflns_theta_min         2.579
_diffrn_ambient_temperature      350.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  IMS_Mo
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          none
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                766
_reflns_number_total             907
_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       'SAINT V8.40A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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         0.134
_refine_diff_density_min         -0.221
_refine_diff_density_rms         0.031
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         907
_refine_ls_number_restraints     60
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0249
_refine_ls_restrained_S_all      1.113
_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)+(0.0374P)²+1.2539P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0691
_refine_ls_wR_factor_ref         0.0749
_refine_special_details          none
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H) groups, All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C3 \\sim C4 \\sim C5 \\sim C4A \\sim C3A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C5) = Uanis(C5A)
3. Rigid body (RIGU) restrains
 C3, C4, C5, C4A, C3A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Others
 Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(C3A)=
 Sof(H3AA)=Sof(H3AB)=0.5*(1-FVAR(2))
 Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C5)=Sof(H5A)=Sof(H5B)=
 Sof(H5C)=0.5*FVAR(2)
 Fixed Sof: N3(0.35) C2(0.16667) H2(0.5) N3A(0.15)
5.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C3(H3A,H3B), C4A(H4AA,H4AB), C3A(H3AA,H3AB)
5.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C5A(H5AA,H5AB,H5AC)
;
_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
Co1 Co 0.333333 0.666667 0.666667 0.04684(16) Uani 1 6 d S T P . .
N1 N 0.666667 0.333333 0.583333 0.0734(9) Uani 1 6 d S T P . .
N2 N 0.47818(11) 0.67988(12) 0.61461(7) 0.0733(4) Uani 1 1 d . . . . .
C1 C 0.56886(13) 0.69266(12) 0.59936(7) 0.0681(4) Uani 1 1 d . . . . .
N3 N 0.666667 0.6892(7) 0.583333 0.090(5) Uani 0.7 2 d S T P C .
C4 C 0.4860(8) 0.3728(10) 0.6015(6) 0.092(2) Uani 0.302(7) 1 d . U . A -2
H4A H 0.510262 0.356371 0.639155 0.110 Uiso 0.302(7) 1 calc R . . A -2
H4B H 0.508026 0.458292 0.602923 0.110 Uiso 0.302(7) 1 calc R . . A -2
C3 C 0.5801(7) 0.3727(9) 0.5594(6) 0.093(2) Uani 0.302(7) 1 d . U . A -2
H3A H 0.536076 0.319399 0.526815 0.111 Uiso 0.302(7) 1 calc R . . A -2
H3B H 0.628866 0.454829 0.543776 0.111 Uiso 0.302(7) 1 calc R . . A -2
C5 C 0.349(2) 0.306(3) 0.6050(9) 0.114(4) Uani 0.302(7) 1 d . U . A -2
H5A H 0.321256 0.364298 0.604470 0.171 Uiso 0.302(7) 1 calc GR . . A -2
H5B H 0.323426 0.259677 0.640521 0.171 Uiso 0.302(7) 1 calc GR . . A -2
H5C H 0.315797 0.252120 0.572084 0.171 Uiso 0.302(7) 1 calc GR . . A -2
C2 C 0.666667 0.333333 0.5148(5) 0.160(6) Uani 0.5 3 d S T P A 1
C5A C 0.361(4) 0.322(6) 0.581(4) 0.114(4) Uani 0.198(7) 1 d . . . A -3
H5AA H 0.311615 0.282829 0.547531 0.171 Uiso 0.198(7) 1 calc GR . . A -3
H5AB H 0.348669 0.387986 0.593399 0.171 Uiso 0.198(7) 1 calc GR . . A -3
H5AC H 0.339456 0.264200 0.612352 0.171 Uiso 0.198(7) 1 calc GR . . A -3
C4A C 0.4913(15) 0.3720(17) 0.5661(11) 0.106(3) Uani 0.198(7) 1 d . U . A -3
H4AA H 0.503331 0.405549 0.526881 0.128 Uiso 0.198(7) 1 calc R . . A -3
H4AB H 0.539207 0.439968 0.592244 0.128 Uiso 0.198(7) 1 calc R . . A -3
C3A C 0.5392(13) 0.2992(15) 0.5675(9) 0.096(3) Uani 0.198(7) 1 d . U . A -3
H3AA H 0.525987 0.263453 0.528733 0.116 Uiso 0.198(7) 1 calc R . . A -3
H3AB H 0.487137 0.232738 0.593634 0.116 Uiso 0.198(7) 1 calc R . . A -3
H2 H 0.628(5) 0.403(5) 0.504(3) 0.145 Uiso 0.5 1 d R . . B 1
N3A N 0.640(3) 0.695(3) 0.5588(15) 0.068(5) Uani 0.15 1 d . . . C 1


_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 N2 2.1162(12) 25_566 ?
Co1 N2 2.1161(12) . ?
Co1 N2 2.1161(12) 26_456 ?
Co1 N2 2.1162(12) 27_556 ?
Co1 N2 2.1161(12) 2_665 ?
Co1 N2 2.1161(12) 3_565 ?
N1 C3 1.510(8) . ?
N1 C2 1.566(12) . ?
N1 C2 1.566(12) 16_545 ?
N1 C3A 1.486(13) . ?
N2 C1 1.1275(18) . ?
C1 N3 1.308(5) . ?
C1 N3A 1.28(3) . ?
C1 N3A 1.43(4) 18_655 ?
N3 N3A 0.67(3) . ?
N3 N3A 0.67(3) 18_655 ?
C4 C3 1.529(17) . ?
C4 C5 1.49(2) . ?
C5A C4A 1.47(4) . ?
C4A C3A 1.33(2) . ?
N3A N3A 1.26(7) 18_655 ?

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
N2 Co1 N2 91.45(6) 25_566 27_556 ?
N2 Co1 N2 91.46(6) 2_665 3_565 ?
N2 Co1 N2 88.54(6) 26_456 . ?
N2 Co1 N2 88.54(6) 25_566 2_665 ?
N2 Co1 N2 88.54(6) 27_556 . ?
N2 Co1 N2 88.54(6) 27_556 2_665 ?
N2 Co1 N2 180.0 27_556 3_565 ?
N2 Co1 N2 91.46(6) 25_566 26_456 ?
N2 Co1 N2 88.54(6) 26_456 3_565 ?
N2 Co1 N2 91.46(6) 27_556 26_456 ?
N2 Co1 N2 91.46(6) 2_665 . ?
N2 Co1 N2 180.00(7) 2_665 26_456 ?
N2 Co1 N2 91.46(6) 3_565 . ?
N2 Co1 N2 88.54(6) 25_566 3_565 ?
N2 Co1 N2 180.0 25_566 . ?
C2 N1 C2 180.0 16_545 . ?
C1 N2 Co1 163.60(15) . . ?
N2 C1 N3 171.0(4) . . ?
N2 C1 N3A 153.7(13) . 18_655 ?
N2 C1 N3A 151.3(15) . . ?
N3 C1 N3A 28.0(10) . 18_655 ?
N3A C1 N3 30.1(12) . . ?
N3A C1 N3A 55(2) . 18_655 ?
C1 N3 C1 119.4(7) 18_655 . ?
N3A N3 C1 86(3) . 18_655 ?
N3A N3 C1 73(3) 18_655 18_655 ?
N3A N3 C1 86(3) 18_655 . ?
N3A N3 C1 73(3) . . ?
N3A N3 N3A 139(6) . 18_655 ?
C5 C4 C3 135.2(13) . . ?
N1 C3 C4 117.4(11) . . ?
C3A C4A C5A 120(3) . . ?
C4A C3A N1 127.3(14) . . ?
C1 N3A C1 112(3) . 18_655 ?
N3 N3A C1 66(3) . 18_655 ?
N3 N3A C1 77(3) . . ?
N3 N3A N3A 21(3) . 18_655 ?
N3A N3A C1 69(3) 18_655 . ?
N3A N3A C1 56(2) 18_655 18_655 ?

_olex2_exptl_crystal_mounting_method 
'piece of suitable crystal mounted on microloop sample holder and transferred to the driffractometer'
_olex2_submission_original_sample_id BurSt120
_olex2_submission_special_instructions 'No special instructions were received'
