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_4088673
_publ_section_title
;
 A Well-Defined Isocyano Analogue of HCo(CO)4. 1: Synthesis,
 Decomposition, and Catalytic 1,1-Hydrogenation of Isocyanides
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_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         'C84 H85 Co N4, (C4 H10 O)'
_chemical_formula_sum            'C90 H100 Co N4 O'
_chemical_formula_weight         1246.54
_chemical_name_common            Co(H)(CNArMes2)3(XylNC)
_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
_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                104.196(8)
_cell_angle_beta                 90.338(9)
_cell_angle_gamma                116.827(8)
_cell_formula_units_Z            2
_cell_length_a                   13.365(4)
_cell_length_b                   14.291(4)
_cell_length_c                   21.974(5)
_cell_measurement_reflns_used    2837
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      20.48
_cell_measurement_theta_min      2.43
_cell_volume                     3597.8(17)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_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)'
_diffrn_ambient_temperature      90.0
_diffrn_measured_fraction_theta_full 0.779
_diffrn_measured_fraction_theta_max 0.734
_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  0.0536
_diffrn_reflns_av_unetI/netI     0.0910
_diffrn_reflns_Laue_measured_fraction_full 0.779
_diffrn_reflns_Laue_measured_fraction_max 0.734
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            24692
_diffrn_reflns_point_group_measured_fraction_full 0.779
_diffrn_reflns_point_group_measured_fraction_max 0.734
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.563
_diffrn_reflns_theta_min         1.662
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.286
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6719
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0508 before and 0.0442 after correction.
The Ratio of minimum to maximum transmission is 0.9016.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1330
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     825
_refine_ls_number_reflns         9900
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1172
_refine_ls_R_factor_gt           0.0612
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0740P)^2^+1.4786P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1338
_refine_ls_wR_factor_ref         0.1563
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6145
_reflns_number_total             9900
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00297_si_002.cif
_cod_data_source_block           jfig642_0m_sq
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        3597.8(16)
_cod_original_formula_sum        'C90 H100 Co N4 O1'
_cod_database_code               4088673
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.945
_platon_squeeze_void_probe_radius 1.20
_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
 C11A-C12A
 1.4 with sigma of 0.02
3. Restrained planarity
 C5A, C6A, C7A, C8A, C11A, C12A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C7B) = Uanis(C7A)
Uanis(C5B) = Uanis(C5A) = Uanis(C6B) = Uanis(C6A) = Uanis(C8A) = Uanis(C8B) =
Uanis(C9A) = Uanis(C9B) = Uanis(C10A) = Uanis(C10B) = Uanis(C11A)
Uanis(C12A) = Uanis(C12B)
Uanis(C57) = Uanis(C57B)
Uanis(C56) = Uanis(C56B)
5. Others
 Sof(C5A)=Sof(C11A)=Sof(C10A)=Sof(H10A)=Sof(C9A)=Sof(H9A)=Sof(C8A)=Sof(H8A)=
 Sof(C6A)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=Sof(C12A)=Sof(H12A)=Sof(H12B)=
 Sof(H12C)=1-FVAR(1)
 Sof(C5B)=Sof(C6B)=Sof(C7B)=Sof(H7BA)=Sof(H7BB)=Sof(H7BC)=Sof(C8B)=Sof(H8B)=
 Sof(C9B)=Sof(H9B)=Sof(C10B)=Sof(H10B)=Sof(C11B)=Sof(C12B)=Sof(H12D)=Sof(H12E)=
 Sof(H12F)=FVAR(1)
 Sof(H55A)=Sof(C56B)=Sof(C57B)=Sof(H57D)=Sof(H57E)=Sof(H57F)=Sof(H58A)=1-FVAR(2)
 Sof(H55)=Sof(C56)=Sof(C57)=Sof(H57A)=Sof(H57B)=Sof(H57C)=Sof(H58)=FVAR(2)
6.a Aromatic/amide H refined with riding coordinates:
 C10A(H10A), C9A(H9A), C8A(H8A), C8B(H8B), C9B(H9B), C10B(H10B), C15(H15),
 C16(H16), C17(H17), C22(H22), C25(H25), C31(H31), C34(H34), C39(H39), C40(H40),
  C41(H41), C46(H46), C49(H49), C55(H55), C55(H55A), C58(H58), C58(H58A),
 C63(H63), C64(H64), C65(H65), C70(H70), C73(H73), C79(H79), C82(H82)
6.b Fitted hexagon refined as free rotating group:
 C5A(C11A,C10A,C9A,C8A,C6A)
6.c Idealised Me refined as rotating group:
 C7A(H7AA,H7AB,H7AC), C7B(H7BA,H7BB,H7BC), C12A(H12A,H12B,H12C), C12B(H12D,
 H12E,H12F), C21(H21A,H21B,H21C), C24(H24A,H24B,H24C), C27(H27A,H27B,H27C),
 C30(H30A,H30B,H30C), C33(H33A,H33B,H33C), C36(H36A,H36B,H36C), C45(H45A,H45B,
 H45C), C48(H48A,H48B,H48C), C51(H51A,H51B,H51C), C54(H54A,H54B,H54C), C57(H57A,
 H57B,H57C), C57B(H57D,H57E,H57F), C60(H60A,H60B,H60C), C69(H69A,H69B,H69C),
 C72(H72A,H72B,H72C), C75(H75A,H75B,H75C), C78(H78A,H78B,H78C), C81(H81A,H81B,
 H81C), C84(H84A,H84B,H84C)
;
_shelx_res_checksum              47526
_shelx_hkl_checksum              65858
_shelx_fab_checksum              4084
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'