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_7716086
_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_formula_moiety         'C44 H66 Br2 Co2 N8 O4, 2(Cl O4), 3[CH4O]'
_chemical_formula_sum            'C47 H78 Br2 Cl2 Co2 N8 O15'
_chemical_formula_weight         1343.75
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-03-29
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.12.21 svn.raa29eb21 for OlexSys, GUI svn.r6440)
;
_audit_update_record
;
2024-03-18 deposited with the CCDC.	2024-05-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.4700(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.7597(14)
_cell_length_b                   14.4732(6)
_cell_length_c                   24.5591(8)
_cell_measurement_reflns_used    9810
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.730
_cell_measurement_theta_min      2.178
_cell_volume                     11848.3(8)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'APEX4 v2021.10-0 (Bruker AXS, 2021)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-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 1.000
_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  0.0444
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            131671
_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         30.034
_diffrn_reflns_theta_min         1.534
_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    2.067
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.5987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0684 before and 0.0448 after correction.
The Ratio of minimum to maximum transmission is 0.8023.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_description       plate
_exptl_crystal_F_000             5552
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.836
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     721
_refine_ls_number_reflns         17357
_refine_ls_number_restraints     234
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0369P)^2^+25.5648P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.0905
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13535
_reflns_number_total             17357
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00877d2.cif
_cod_data_source_block           g2793
_cod_depositor_comments
'Adding full bibliography for 7716081--7716089.cif.'
_cod_database_code               7716086
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.859
_shelx_estimated_absorpt_t_min   0.568
_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
 Cl3-O33 \\sim Cl3-O34B \\sim Cl3-O34 \\sim Cl3-O31 \\sim Cl3-O32 \\sim Cl3-O33B
 with sigma of 0.02
 Cl4-O43B \\sim Cl4-O43 \\sim Cl4-O42 \\sim Cl4-O42B \\sim Cl4-O41 \\sim
Cl4-O44 \\sim Cl4-O44B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O31 \\sim O32 \\sim O33 \\sim O33B \\sim O34 \\sim O34B: within 2.5A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 2.5A
O41 \\sim O42 \\sim O42B \\sim O43 \\sim O43B \\sim O44 \\sim O44B: within 2.5A
with sigma of 0.04 and sigma for terminal atoms of 0.06 within 2.5A
4. Others
 Sof(O42B)=Sof(O43B)=Sof(O44B)=1-FVAR(1)
 Sof(O42)=Sof(O43)=Sof(O44)=FVAR(1)
 Sof(O33B)=Sof(O34B)=1-FVAR(2)
 Sof(O33)=Sof(O34)=FVAR(2)
 Fixed Sof: O8(0.5) O8B(0.5) C12(0.5) H12A(0.5) H12B(0.5) H12C(0.5) C12B(0.5)
 H12D(0.5) H12E(0.5) H12F(0.5) C21(0.5) H21A(0.5) H21B(0.5) H21C(0.5) C21B(0.5)
 H21D(0.5) H21E(0.5) H21F(0.5)
5.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)
5.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C30(H30), C50(H50), C70(H70)
5.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C12B(H12D,H12E,
 H12F), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,
 H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C),
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C21B(H21D,H21E,H21F), C22(H22A,H22B,
 H22C), C44(H44A,H44B,H44C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 428 electrons were 
found in a volume of 1992\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
0.5[CH4O], 2.5[CH4O] per Formula Unit 
which account for 432 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              4366
_shelx_fab_checksum              72449
_olex2_submission_special_instructions 'No special instructions were received'