Side-On Coordination of Nitrous Oxide to a Mononuclear Cobalt Center.
Mokhtarzadeh, Charles C.; Chan, Chinglin; Moore, Curtis E.; Rheingold, Arnold L.; Figueroa, Joshua S.; Journal of the American Chemical Society 141 (2019) 15003–15007; doi:10.1021/jacs.9b08241

data_4129007
_publ_section_title
;
 Side-On Coordination of Nitrous Oxide to a Mononuclear Cobalt Center.
;
_journal_issue                   38
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15003
_journal_page_last               15007
_journal_paper_doi               10.1021/jacs.9b08241
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C65 H79 Co N P'
_chemical_formula_sum            'C65 H79 Co N P'
_chemical_formula_weight         964.19
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2016-09-03
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
_audit_update_record
;
2016-09-19 # Formatted by publCIF

;
_cell_angle_alpha                90
_cell_angle_beta                 90.367(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5984(11)
_cell_length_b                   17.6290(12)
_cell_length_c                   23.0085(18)
_cell_measurement_reflns_used    2147
_cell_measurement_temperature    100
_cell_measurement_theta_max      21.191
_cell_measurement_theta_min      2.474
_cell_volume                     5515.6(7)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2013.6-2 (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker APEX CCD'
_diffrn_detector_area_resol_mean 8.0
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker X8 APEX'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0839
_diffrn_reflns_av_unetI/netI     0.1290
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25806
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.327
_diffrn_reflns_theta_min         2.312
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.380
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6352
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0540 before and 0.0485 after correction.
The Ratio of minimum to maximum transmission is 0.8524.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'dull dark orange'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.161
_exptl_crystal_description       block
_exptl_crystal_F_000             2072
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.762
_refine_diff_density_min         -0.408
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     630
_refine_ls_number_reflns         10028
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.1271
_refine_ls_R_factor_gt           0.0580
_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^)+(0.0493P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1076
_refine_ls_wR_factor_ref         0.1287
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5841
_reflns_number_total             10028
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b08241_si_002.cif
_cod_data_source_block           jfig1383
_cod_database_code               4129007
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C35(H35), C25(H25), C20(H20), C30(H30), C10(H10), C15(H15)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C53(H53), C61(H61), C28(H28), C55(H55), C62(H62), C33(H33), C59(H59),
 C5(H5), C64(H64), C65(H65), C18(H18), C49(H49), C52(H52), C58(H58), C63(H63),
 C56(H56), C57(H57), C50(H50), C13(H13), C4(H4), C51(H51)
2.c Idealised Me refined as rotating group:
 C41(H41A,H41B,H41C), C43(H43A,H43B,H43C), C26(H26A,H26B,H26C), C39(H39A,H39B,
 H39C), C32(H32A,H32B,H32C), C27(H27A,H27B,H27C), C31(H31A,H31B,H31C), C11(H11A,
 H11B,H11C), C47(H47A,H47B,H47C), C37(H37A,H37B,H37C), C21(H21A,H21B,H21C),
 C45(H45A,H45B,H45C), C12(H12A,H12B,H12C), C22(H22A,H22B,H22C), C36(H36A,H36B,
 H36C), C17(H17A,H17B,H17C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              63596
_shelx_hkl_checksum              56381
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'