A Well-Defined Isocyano Analogue of HCo(CO)4. 1: Synthesis, Decomposition, and Catalytic 1,1-Hydrogenation of Isocyanides
Carpenter, Alex E.; Rheingold, Arnold L.; Figueroa, Joshua S.; Organometallics 35 (2016) 2309–; doi:10.1021/acs.organomet.6b00297

data_4088669
_publ_section_title
;
 A Well-Defined Isocyano Analogue of HCo(CO)4. 1: Synthesis,
 Decomposition, and Catalytic 1,1-Hydrogenation of Isocyanides
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              2309
_journal_paper_doi               10.1021/acs.organomet.6b00297
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         '0.5(C50 H51.5 Co N2), 0.25(C50 H51 Co N2)'
_chemical_formula_sum            'C37.5 H38.5 Co0.75 N1.5'
_chemical_formula_weight         554.39
_chemical_melting_point          ?
_chemical_name_common            Co(HCNArMes2)(CNArMEs2)
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-02-22
_audit_creation_method
; 
Olex2 1.2 
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998) 
;
_cell_angle_alpha                94.906(3)
_cell_angle_beta                 106.630(3)
_cell_angle_gamma                110.407(2)
_cell_formula_units_Z            4
_cell_length_a                   11.3496(5)
_cell_length_b                   15.7745(7)
_cell_length_c                   18.5671(8)
_cell_measurement_reflns_used    9968
_cell_measurement_temperature    90
_cell_measurement_theta_max      30.63
_cell_measurement_theta_min      2.47
_cell_volume                     2921.0(2)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 8.0
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0513
_diffrn_reflns_av_unetI/netI     0.0616
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            63119
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.822
_diffrn_reflns_theta_min         1.408
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.478
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.7138
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS-2008/1 (Bruker,2008) was used for absorption correction. 
wR2(int) was 0.0493 before and 0.0458 after correction. 
The Ratio of minimum to maximum transmission is 0.9567. 
The \l/2 correction factor is 0.0015. 
;
_exptl_crystal_colour            'Dark red'
_exptl_crystal_colour_lustre     Dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plates
_exptl_crystal_F_000             1177
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.575
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     780
_refine_ls_number_reflns         17921
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0890
_refine_ls_R_factor_gt           0.0548
_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^)+(0.0511P)^2^+1.7801P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1236
_refine_ls_wR_factor_ref         0.1368
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12469
_reflns_number_total             17921
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00297_si_002.cif
_cod_data_source_block           jfig596_0m_CoLHL
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value 'not measured' was changed
to '?' -- the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_formula_sum        'C37.50 H38.50 Co0.75 N1.50'
_cod_database_code               4088669
_shelx_estimated_absorpt_t_max   0.954
_shelx_estimated_absorpt_t_min   0.832
_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. Uiso/Uaniso restraints and constraints 
Uanis(C51) = Uanis(C52) 
3. Others 
 Sof(C2B)=1-FVAR(1) 
 Sof(C1A)=FVAR(1) 
 Sof(C2A)=1-FVAR(2) 
 Sof(C1B)=FVAR(2) 
 Sof(Co1A)=1-FVAR(3) 
 Sof(Co1B)=FVAR(3) 
 Fixed Sof: H1A(0.5) C51(0.5) H51(0.5) C52(0.5) Co2(0.5) 
4.a Aromatic/amide H refined with riding coordinates: 
 C5(H5), C6(H6), C7(H7), C12(H12), C15(H15), C21(H21), C24(H24), C29(H29), 
 C30(H30), C31(H31), C36(H36), C39(H39), C45(H45), C48(H48), C55(H55), C56(H56), 
  C57(H57), C62(H62), C65(H65), C71(H71), C74(H74), C51(H51) 
4.b Idealised Me refined as rotating group: 
 C11(H11A,H11B,H11C), C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C20(H20A,H20B, 
 H20C), C23(H23A,H23B,H23C), C26(H26A,H26B,H26C), C35(H35A,H35B,H35C), C38(H38A, 
 H38B,H38C), C41(H41A,H41B,H41C), C44(H44A,H44B,H44C), C47(H47A,H47B,H47C), 
 C50(H50A,H50B,H50C), C61(H61A,H61B,H61C), C64(H64A,H64B,H64C), C67(H67A,H67B, 
 H67C), C70(H70A,H70B,H70C), C73(H73A,H73B,H73C), C76(H76A,H76B,H76C) 
;
_shelx_res_checksum              75414
_shelx_hkl_checksum              35391
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'