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_4088676
_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         'C77 H76 Co N3 O2, C5 H12'
_chemical_formula_sum            'C82 H88 Co N3 O2'
_chemical_formula_weight         1206.48
_chemical_melting_point          ?
_chemical_name_common            (HCNArMes2)Co(CNArMes2)2(CO)2
_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   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                90
_cell_angle_beta                 106.846(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.424(2)
_cell_length_b                   14.2969(12)
_cell_length_c                   26.503(2)
_cell_measurement_reflns_used    4531
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.031
_cell_measurement_theta_min      2.542
_cell_volume                     7044.1(11)
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 8.0
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.1494
_diffrn_reflns_av_unetI/netI     0.1731
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            32380
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        22.030
_diffrn_reflns_theta_max         22.030
_diffrn_reflns_theta_min         1.635
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.291
_exptl_absorpt_correction_T_max  0.7447
_exptl_absorpt_correction_T_min  0.5906
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0787 before and 0.0682 after correction.
The Ratio of minimum to maximum transmission is 0.7931.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2576
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.280
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     829
_refine_ls_number_reflns         8617
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.1591
_refine_ls_R_factor_gt           0.0646
_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^)+(0.0583P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1205
_refine_ls_wR_factor_ref         0.1525
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4519
_reflns_number_total             8617
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00297_si_002.cif
_cod_data_source_block           jfig547_0m
_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_database_code               4088676
_shelx_estimated_absorpt_t_max   0.971
_shelx_estimated_absorpt_t_min   0.944
_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. Uiso/Uaniso restraints and constraints
Uanis(N1) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C2SB) = Uanis(C2SA) = Uanis(C3SA) = Uanis(C3SB) = Uanis(C4SB) =
Uanis(C4SA)
Uanis(N1) = Uanis(N2) = Uanis(N3)
3. Rigid body (RIGU) restrains
 C1SA, C1SB, C2SB, C2SA, C3SA, C3SB, C4SB, C4SA, C5SA, C5SB
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: C1SB(0.25) H1SA(0.25) H1SB(0.25) H1SC(0.25) C2SB(0.25) H2SA(0.25)
 H2SB(0.25) C3SB(0.25) H3SA(0.25) H3SB(0.25) C4SB(0.25) H4SA(0.25) H4SB(0.25)
 C5SB(0.25) H5SA(0.25) H5SB(0.25) H5SC(0.25) C5SA(0.75) H5SD(0.75) H5SE(0.75)
 H5SF(0.75) C2SA(0.75) H2SC(0.75) H2SD(0.75) C1SA(0.75) H1SD(0.75) H1SE(0.75)
 H1SF(0.75) C4SA(0.75) H4SC(0.75) H4SD(0.75) C3SA(0.75) H3SC(0.75) H3SD(0.75)
5.a Secondary CH2 refined with riding coordinates:
 C2SB(H2SA,H2SB), C3SB(H3SA,H3SB), C4SB(H4SA,H4SB), C2SA(H2SC,H2SD), C4SA(H4SC,
 H4SD), C3SA(H3SC,H3SD)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C8(H8), C9(H9), C10(H10), C15(H15), C18(H18), C24(H24), C27(H27),
 C32(H32), C33(H33), C34(H34), C39(H39), C42(H42), C48(H48), C51(H51), C56(H56),
  C57(H57), C58(H58), C63(H63), C66(H66), C72(H72), C75(H75)
5.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C20(H20A,H20B,H20C), C23(H23A,H23B,H23C), C26(H26A,H26B,
 H26C), C29(H29A,H29B,H29C), C38(H38A,H38B,H38C), C41(H41A,H41B,H41C), C44(H44A,
 H44B,H44C), C47(H47A,H47B,H47C), C50(H50A,H50B,H50C), C53(H53A,H53B,H53C),
 C62(H62A,H62B,H62C), C65(H65A,H65B,H65C), C68(H68A,H68B,H68C), C71(H71A,H71B,
 H71C), C74(H74A,H74B,H74C), C77(H77A,H77B,H77C), C1SB(H1SA,H1SB,H1SC),
 C5SB(H5SA,H5SB,H5SC), C5SA(H5SD,H5SE,H5SF), C1SA(H1SD,H1SE,H1SF)
;
_shelx_res_checksum              43194
_shelx_hkl_checksum              33145
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'