Crystal Structure and C-H Bond Cleaving Reactivity of a Mononuclear Co<sup>IV</sup>-dinitrate Complex.
Kwon, Yubin M.; Lee, Yuri; Evenson, Garrett E.; Jackson, Timothy A.; Wang, Dong; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c04368

data_4135120
_publ_section_title
;
 Crystal Structure and C-H Bond Cleaving Reactivity of a Mononuclear
 Co<sup>IV</sup>-dinitrate Complex.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c04368
_journal_year                    2020
_chemical_formula_moiety         'C27 H33 Co N4 O3, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C27.5 H34 Cl Co N4 O3'
_chemical_formula_weight         562.96
_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
_audit_creation_date             2020-02-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 116.4340(10)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   36.2527(18)
_cell_length_b                   10.9071(5)
_cell_length_c                   30.0533(15)
_cell_measurement_reflns_used    9560
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.308
_cell_measurement_theta_min      2.605
_cell_volume                     10641.0(9)
_computing_cell_refinement       'SAINT V8.38A (BRUKER-AXS, 2016)'
_computing_data_collection       'APEX3 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT V8.38A (BRUKER-AXS, 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)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker Photon-100 area detector'
_diffrn_detector_area_resol_mean 10.5
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'Fixed Chi Three-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE Duo'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'TRIUMPH graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0737
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            153636
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.441
_diffrn_reflns_theta_min         2.510
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.782
_exptl_absorpt_correction_T_max  0.6937
_exptl_absorpt_correction_T_min  0.6213
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0619 before and 0.0567 after correction. The Ratio of minimum to maximum transmission is 0.8956. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_description       plate
_exptl_crystal_F_000             4720
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.775
_refine_diff_density_min         -0.960
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     674
_refine_ls_number_reflns         9826
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0463
_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^)+(0.0510P)^2^+40.1313P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1099
_refine_ls_wR_factor_ref         0.1201
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7624
_reflns_number_total             9826
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c04368_si_004.cif
_cod_data_source_block           umt_dw66
_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/ACS/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 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_formula_sum        'C27.50 H34 Cl Co N4 O3'
_cod_database_code               4135120
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.985
_shelx_estimated_absorpt_t_min   0.817
_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.a Secondary CH2 refined with riding coordinates:
 C1C(H1CA,H1CB)
2.b Aromatic/amide H refined with riding coordinates:
 C2B(H2B), C3B(H3B), C4B(H4B), C11B(H11B), C12B(H12B), C13B(H13B), C22B(H22B),
 C23B(H23B), C24B(H24B), C2A(H2A), C3A(H3A), C4A(H4A), C11A(H11A), C12A(H12A),
 C13A(H13A), C22A(H22A), C23A(H23A), C24A(H24A)
2.c Idealised Me refined as rotating group:
 C7B(H7BA,H7BB,H7BC), C8B(H8BA,H8BB,H8BC), C15B(H15A,H15B,H15C), C16B(H16A,
 H16B,H16C), C18B(H18A,H18B,H18C), C19B(H19A,H19B,H19C), C26B(H26A,H26B,H26C),
 C27B(H27A,H27B,H27C), C7A(H7AA,H7AB,H7AC), C8A(H8AA,H8AB,H8AC), C15A(H15D,H15E,
 H15F), C16A(H16D,H16E,H16F), C18A(H18D,H18E,H18F), C19A(H19D,H19E,H19F),
 C26A(H26D,H26E,H26F), C27A(H27D,H27E,H27F)
;
_shelx_res_checksum              18014
_shelx_hkl_checksum              71916
_olex2_submission_special_instructions 'No special instructions were received'