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_4129003
_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         'C47 H64 Co N3'
_chemical_formula_sum            'C47 H64 Co N3'
_chemical_formula_weight         729.94
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-24
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.07.08 svn.r3312 for OlexSys, GUI svn.r5203)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.4002(4)
_cell_length_b                   20.7307(5)
_cell_length_c                   23.4789(6)
_cell_measurement_reflns_used    9916
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.31
_cell_volume                     8469.3(4)
_computing_cell_refinement       'SAINT v8.34A (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, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0460
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            42884
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.762
_diffrn_reflns_theta_max         25.762
_diffrn_reflns_theta_min         1.735
_diffrn_source                   'Cu Rotating Anode'
_diffrn_source_target            Mo
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.439
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6837
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0738 before and 0.0442 after correction. The Ratio of minimum to maximum transmission is 0.9173. 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    1.145
_exptl_crystal_description       plate
_exptl_crystal_F_000             3152
_exptl_crystal_size_max          0.84
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.853
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     477
_refine_ls_number_reflns         8045
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0633
_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^)+(0.0639P)^2^+15.3065P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1493
_refine_ls_wR_factor_ref         0.1613
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6093
_reflns_number_total             8045
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b08241_si_002.cif
_cod_data_source_block           JFig1291
_cod_database_code               4129003
_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:
 C25(H25), C29(H29), C15(H15), C10(H10), C20(H20), C34(H34)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C37(H37), C5(H5), C32(H32), C13(H13), C6(H6), C18(H18)
2.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C43(H43A,H43B,H43C), C41(H41A,H41B,H41C), C31(H31A,H31B,
 H31C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C39(H39A,H39B,H39C), C30(H30A,
 H30B,H30C), C27(H27A,H27B,H27C), C45(H45A,H45B,H45C), C22(H22A,H22B,H22C),
 C16(H16A,H16B,H16C), C47(H47A,H47B,H47C), C26(H26A,H26B,H26C), C21(H21A,H21B,
 H21C), C36(H36A,H36B,H36C), C35(H35A,H35B,H35C)
;
_shelx_res_checksum              26597
_shelx_hkl_checksum              94636
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'