Increasing the electron donation in a dinucleating ligand family: molecular and electronic structures in a series of Co<sup>II</sup>Co<sup>II</sup> complexes.
Depenbrock, Felix; Limpke, Thomas; Stammler, Anja; Oldengott, Jan; Bögge, Hartmut; Glaser, Thorsten; Dalton transactions (Cambridge, England : 2003) 53 (2024) 9554–9567; doi:10.1039/d4dt00877d

data_7716088
_publ_section_title
;
 Increasing the electron donation in a dinucleating ligand family:
 molecular and electronic structures in a series of
 Co<sup>II</sup>Co<sup>II</sup> complexes.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9554
_journal_page_last               9567
_journal_paper_doi               10.1039/d4dt00877d
_journal_volume                  53
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C28 H46 Br2 Co2 N12, 2(Cl O4)'
_chemical_formula_sum            'C28 H46 Br2 Cl2 Co2 N12 O8'
_chemical_formula_weight         1027.35
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-09-13
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2024-03-18 deposited with the CCDC.	2024-05-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4043(6)
_cell_length_b                   13.0584(7)
_cell_length_c                   24.6003(11)
_cell_measurement_reflns_used    9696
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.200
_cell_measurement_theta_min      2.265
_cell_volume                     3984.8(3)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'APEX3 v2016.5-0 (Bruker AXS, 2016)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/1 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker APEX II area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker KAPPA APEX Duo'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'graphite monochromator'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0129
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            246620
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.949
_diffrn_reflns_theta_min         1.766
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_type              'Bruker KAPPA APEX Duo'
_diffrn_source_voltage           50.0
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.034
_exptl_absorpt_correction_T_max  0.5657
_exptl_absorpt_correction_T_min  0.4753
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0604 before and 0.0410 after correction.
The Ratio of minimum to maximum transmission is 0.8402.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_description       column
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.765
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details
;
 Flack x determined using 5821 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.0069(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     521
_refine_ls_number_reflns         14231
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0211
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0285P)^2^+1.6174P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0508
_refine_ls_wR_factor_ref         0.0515
_reflns_Friedel_coverage         0.793
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.930
_reflns_number_gt                13612
_reflns_number_total             14231
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00877d2.cif
_cod_data_source_block           g2763
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7716081--7716089.cif.
;
_cod_database_code               7716088
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.611
_shelx_estimated_absorpt_t_min   0.384
_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. Restrained distances
 Cl2-O22B \\sim Cl2-O22 \\sim Cl2-O24B \\sim Cl2-O23 \\sim Cl2-O23B \\sim
Cl2-O24 \\sim Cl2-O21
 with sigma of 0.01
3. Others
 Sof(O22B)=Sof(O23B)=Sof(O24B)=1-FVAR(1)
 Sof(O22)=Sof(O23)=Sof(O24)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C5(H5A,H5B), C25(H25A,H25B), C41(H41A,
 H41B), C42(H42A,H42B), C43(H43A,H43B), C45(H45A,H45B), C65(H65A,H65B)
4.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C28(H28), C29(H29), C48(H48), C49(H49), C68(H68), C69(H69)
4.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C17(H17A,H17B,H17C), C37(H37A,H37B,H37C), C44(H44A,H44B,
 H44C), C57(H57A,H57B,H57C), C77(H77A,H77B,H77C)
;
_shelx_res_checksum              7077
_olex2_submission_special_instructions 'No special instructions were received'