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_4088667
_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         'C100 H101 Co N4, 2(C5 H12)'
_chemical_formula_sum            'C110 H125 Co N4'
_chemical_formula_weight         1562.06
_chemical_melting_point          ?
_chemical_name_common            Co(H)(CNArMes2)4
_chemical_name_systematic
hydridotetrakis(2,6-dimesitylphenylioscyanide)cobalt
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-02-21
_audit_creation_method
; 
Olex2 1.2 
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998) 
;
_cell_angle_alpha                90
_cell_angle_beta                 111.766(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.856(3)
_cell_length_b                   11.6893(11)
_cell_length_c                   27.498(3)
_cell_measurement_reflns_used    2567
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.36
_cell_volume                     8912.5(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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      100.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_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  0.0985
_diffrn_reflns_av_unetI/netI     0.1058
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            52452
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.443
_diffrn_reflns_theta_min         1.469
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.244
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'lusterous yellow orange'
_exptl_crystal_colour_lustre     lusterous
_exptl_crystal_colour_modifier   yellow
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3360
_exptl_crystal_recrystallization_method 'Crystalized from C5/Toluene at -35 C'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.575
_refine_diff_density_min         -0.905
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         9141
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0945
_refine_ls_R_factor_gt           0.0564
_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^)+(0.0552P)^2^+8.7053P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1455
_refine_ls_wR_factor_ref         0.1680
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6398
_reflns_number_total             9141
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00297_si_002.cif
_cod_data_source_block           jfig487
_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.

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        8912.7(14)
_cod_database_code               4088667
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.976
_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(C3SA) \\sim Ueq, Uanis(C3SB) \\sim Ueq: with sigma of 0.1 and sigma for 
terminal atoms of 0.2 
3. Rigid body (RIGU) restrains 
 C2SA, C4SA 
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 
 C3SA, C3SB 
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 
4. Others 
 Sof(C4SB)=Sof(H4SC)=Sof(H4SD)=Sof(C2SB)=Sof(H2SC)=Sof(H2SD)=Sof(C5SB)= 
 Sof(H5SD)=Sof(H5SE)=Sof(H5SF)=Sof(C1SB)=Sof(H1SD)=Sof(H1SE)=Sof(H1SF)= 
 Sof(C3SB)=Sof(H3SC)=Sof(H3SD)=1-FVAR(1) 
 Sof(C3SA)=Sof(H3SA)=Sof(H3SB)=Sof(C1SA)=Sof(H1SA)=Sof(H1SB)=Sof(H1SC)= 
 Sof(C2SA)=Sof(H2SA)=Sof(H2SB)=Sof(C5SA)=Sof(H5SA)=Sof(H5SB)=Sof(H5SC)= 
 Sof(C4SA)=Sof(H4SA)=Sof(H4SB)=FVAR(1) 
 Fixed Sof: H(0.5) 
5.a Secondary CH2 refined with riding coordinates: 
 C3SA(H3SA,H3SB), C4SB(H4SC,H4SD), C2SB(H2SC,H2SD), C2SA(H2SA,H2SB), C3SB(H3SC, 
 H3SD), C4SA(H4SA,H4SB) 
5.b Aromatic/amide H refined with riding coordinates: 
 C12(H12), C36(H36), C24(H24), C45(H45), C48(H48), C29(H29), C30(H30), 
 C15(H15), C21(H21), C39(H39), C31(H31), C5(H5), C7(H7), C6(H6) 
5.c Idealised Me refined as rotating group: 
 C35(H35A,H35B,H35C), C44(H44A,H44B,H44C), C11(H11A,H11B,H11C), C47(H47A,H47B, 
 H47C), C17(H17A,H17B,H17C), C38(H38A,H38B,H38C), C23(H23A,H23B,H23C), C41(H41A, 
 H41B,H41C), C50(H50A,H50B,H50C), C20(H20A,H20B,H20C), C26(H26A,H26B,H26C), 
 C14(H14A,H14B,H14C), C1SA(H1SA,H1SB,H1SC), C5SB(H5SD,H5SE,H5SF), C1SB(H1SD, 
 H1SE,H1SF), C5SA(H5SA,H5SB,H5SC) 
;
_shelx_res_checksum              4002
_shelx_hkl_checksum              90239
_shelx_shelxl_version_number     2014/7
_olex2_submission_original_sample_id jfig487
_olex2_submission_special_instructions 'No special instructions were received'