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_4129006
_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         'C52.92 H73.89 Co N'
_chemical_formula_sum            'C53 H74 Co N'
_chemical_formula_weight         784.06
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2016-09-19
_audit_creation_method
;
Olex2 1.2
(compiled Jan 19 2015 12:28:14 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-09-19 # Formatted by publCIF

;
_cell_angle_alpha                90
_cell_angle_beta                 105.928(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.8319(19)
_cell_length_b                   13.874(2)
_cell_length_c                   19.914(3)
_cell_measurement_reflns_used    9912
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.28
_cell_measurement_theta_min      2.33
_cell_volume                     4737.6(11)
_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  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33812
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.012
_diffrn_reflns_theta_max         25.012
_diffrn_reflns_theta_min         1.359
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker TXS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.396
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6950
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0641 before and 0.0511 after correction.
The Ratio of minimum to maximum transmission is 0.9326.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.099
_exptl_crystal_description       plate
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.054
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.850
_refine_diff_density_min         -1.509
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.365
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         8321
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.364
_refine_ls_R_factor_all          0.1559
_refine_ls_R_factor_gt           0.1454
_refine_ls_shift/su_max          0.673
_refine_ls_shift/su_mean         0.015
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+60.3650P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3041
_refine_ls_wR_factor_ref         0.3088
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7489
_reflns_number_total             8321
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b08241_si_002.cif
_cod_data_source_block           jfig1382
_cod_original_cell_volume        4737.7(11)
_cod_database_code               4129006
_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
 C31B-C32B
 2.5 with sigma of 0.02
 C31B-C30B
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C37B) \\sim Ueq, Uanis(C35B) \\sim Ueq, Uanis(C36B) \\sim Ueq: with sigma
of 0.1 and sigma for terminal atoms of 0.2
Uanis(C37A) = Uanis(C35A) = Uanis(C36A)
Uanis(C26A) = Uanis(C27A) = Uanis(C25A)
Uanis(C34A) = Uanis(C23A) = Uanis(C28A) = Uanis(C24A) = Uanis(C29A) =
Uanis(C33A)
Uanis(C26B) = Uanis(C25B) = Uanis(C27B)
Uanis(C30B) = Uanis(C31B) = Uanis(C32B)
Uanis(C24B) = Uanis(C28B) = Uanis(C33B) = Uanis(C29B) = Uanis(C34B) =
Uanis(C23B)
Uanis(C35B) = Uanis(C37B) = Uanis(C36B)
Uanis(C32A) = Uanis(C30A) = Uanis(C31A)
Uanis(C32B) = Uanis(C30B) = Uanis(C31B)
Uanis(C30A) = Uanis(C30B)
Uanis(C27B) = Uanis(C36A)
Uanis(C45B) = Uanis(C45A)
Uanis(C40B) = Uanis(C40A)
Uanis(C41A) = Uanis(C41B)
Uanis(C46B) = Uanis(C46A)
Uanis(C42A) = Uanis(C42B)
Uanis(C47B) = Uanis(C47A)
Uanis(C38A) = Uanis(C38B)
Uanis(C43A) = Uanis(C43B)
Uanis(C39A) = Uanis(C39B)
Uanis(C44A) = Uanis(C44B)
4. Others
 Sof(C30B)=Sof(H30B)=1-FVAR(1)
 Sof(C30A)=Sof(H30A)=FVAR(1)
 Sof(C31B)=Sof(H31D)=Sof(H31E)=Sof(H31F)=1-FVAR(2)
 Sof(C31A)=Sof(H31A)=Sof(H31B)=Sof(H31C)=FVAR(2)
 Sof(C32B)=Sof(H32D)=Sof(H32E)=Sof(H32F)=1-FVAR(3)
 Sof(C32A)=Sof(H32A)=Sof(H32B)=Sof(H32C)=FVAR(3)
 Fixed Sof: C41A(0.75) C42A(0.75) C38A(0.75) C39A(0.75) C40A(0.75) C46A(0.75)
 H46A(0.75) H46B(0.75) H46C(0.75) C47A(0.75) H47A(0.75) H47B(0.75) H47C(0.75)
 C43A(0.75) H43A(0.75) H43B(0.75) H43C(0.75) C44A(0.75) H44A(0.75) H44B(0.75)
 H44C(0.75) C45A(0.75) H45A(0.75) H45B(0.75) H45C(0.75) C35A(0.66) H35A(0.66)
 C23A(0.66) C34A(0.66) C24A(0.66) C28A(0.66) H28A(0.66) C37A(0.66) H37A(0.66)
 H37B(0.66) H37C(0.66) C33A(0.66) H33A(0.66) C29A(0.66) C25A(0.66) H25A(0.66)
 C36A(0.66) H36A(0.66) H36B(0.66) H36C(0.66) C26A(0.66) H26A(0.66) H26B(0.66)
 H26C(0.66) C27A(0.66) H27A(0.66) H27B(0.66) H27C(0.66) C26B(0.33333)
 H26D(0.33333) H26E(0.33333) H26F(0.33333) C25B(0.33333) H25B(0.33333)
 C27B(0.33333) H27D(0.33333) H27E(0.33333) H27F(0.33333) C24B(0.33333)
 C28B(0.33333) H28B(0.33333) C23B(0.33333) C34B(0.33333) C33B(0.33333)
 H33B(0.33333) C29B(0.33333) C35B(0.33333) H35B(0.33333) C36B(0.33333)
 H36D(0.33333) H36E(0.33333) H36F(0.33333) C37B(0.33333) H37D(0.33333)
 H37E(0.33333) H37F(0.33333) C39B(0.25) C40B(0.25) C41B(0.25) C42B(0.25)
 C38B(0.25) C44B(0.25) H44D(0.25) H44E(0.25) H44F(0.25) C45B(0.25) H45D(0.25)
 H45E(0.25) H45F(0.25) C46B(0.25) H46D(0.25) H46E(0.25) H46F(0.25) C47B(0.25)
 H47D(0.25) H47E(0.25) H47F(0.25) C43B(0.25) H43D(0.25) H43E(0.25) H43F(0.25)
5.a Ternary CH refined with riding coordinates:
 C10(H10), C48(H48), C49(H49), C20(H20), C15(H15), C35A(H35A), C25A(H25A),
 C30A(H30A), C25B(H25B), C30B(H30B), C35B(H35B)
5.b Secondary CH2 refined with riding coordinates:
 C53(H53A,H53B), C52(H52A,H52B), C51(H51A,H51B), C50(H50A,H50B)
5.c Aromatic/amide H refined with riding coordinates:
 C18(H18), C4(H4), C5(H5), C6(H6), C13(H13), C28A(H28A), C33A(H33A),
 C28B(H28B), C33B(H33B)
5.d Cp* refined as free rotating group:
 C39B(C40B,C41B,C42B,C38B,C44B,C45B,C46B,C47B,C43B)
5.e Idealised Me refined as rotating group:
 C46A(H46A,H46B,H46C), C47A(H47A,H47B,H47C), C43A(H43A,H43B,H43C), C44A(H44A,
 H44B,H44C), C45A(H45A,H45B,H45C), C12(H12A,H12B,H12C), C16(H16A,H16B,H16C),
 C11(H11A,H11B,H11C), C22(H22A,H22B,H22C), C17(H17A,H17B,H17C), C21(H21A,H21B,
 H21C), C37A(H37A,H37B,H37C), C36A(H36A,H36B,H36C), C26A(H26A,H26B,H26C),
 C32A(H32A,H32B,H32C), C27A(H27A,H27B,H27C), C31A(H31A,H31B,H31C), C26B(H26D,
 H26E,H26F), C27B(H27D,H27E,H27F), C31B(H31D,H31E,H31F), C32B(H32D,H32E,H32F),
 C36B(H36D,H36E,H36F), C37B(H37D,H37E,H37F), C44B(H44D,H44E,H44F), C45B(H45D,
 H45E,H45F), C46B(H46D,H46E,H46F), C47B(H47D,H47E,H47F), C43B(H43D,H43E,H43F)
;
_shelx_res_checksum              2496
_shelx_hkl_checksum              31006
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'