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_4088675
_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         'C93 H91 Co N3 P, C3.5 H4'
_chemical_formula_sum            'C96.5 H95 Co N3 P'
_chemical_formula_weight         1386.65
_chemical_melting_point          ?
_chemical_name_common            CoH(PPh3)(CNArMes2)3
_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
_audit_creation_date             2014-08-21
_audit_creation_method
; 
Olex2 1.2-beta 
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862) 
;
_cell_angle_alpha                90
_cell_angle_beta                 94.636(19)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.971(9)
_cell_length_b                   15.184(5)
_cell_length_c                   43.841(15)
_cell_measurement_reflns_used    2887
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.13
_cell_measurement_theta_min      2.422
_cell_volume                     15241(9)
_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    XS
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 8.0
_diffrn_measured_fraction_theta_full 0.689
_diffrn_measured_fraction_theta_max 0.839
_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  0.1063
_diffrn_reflns_av_unetI/netI     0.1805
_diffrn_reflns_Laue_measured_fraction_full 0.689
_diffrn_reflns_Laue_measured_fraction_max 0.839
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            29924
_diffrn_reflns_point_group_measured_fraction_full 0.689
_diffrn_reflns_point_group_measured_fraction_max 0.839
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         23.547
_diffrn_reflns_theta_min         1.895
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.296
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.6092
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS-2008/1 (Bruker,2008) was used for absorption correction. 
wR2(int) was 0.0805 before and 0.0584 after correction. 
The Ratio of minimum to maximum transmission is 0.8178. 
The \l/2 correction factor is 0.0015. 
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             5896
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     942
_refine_ls_number_reflns         9522
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.1698
_refine_ls_R_factor_gt           0.0716
_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^)+(0.0681P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1253
_refine_ls_wR_factor_ref         0.1579
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4938
_reflns_number_total             9522
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00297_si_002.cif
_cod_data_source_block           jfig708_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_original_cell_volume        15242(9)
_cod_original_formula_sum        'C96.50 H95 Co N3 P'
_cod_database_code               4088675
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.997
_shelx_estimated_absorpt_t_min   0.943
_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. Others 
 Fixed Sof: C1S(0.5) H1SA(0.5) H1SB(0.5) H1SC(0.5) H2S(0.5) 
3.a Aromatic/amide H refined with riding coordinates: 
 C6(H6), C7(H7), C8(H8), C13(H13), C16(H16), C22(H22), C25(H25), C30(H30), 
 C31(H31), C32(H32), C37(H37), C40(H40), C46(H46), C49(H49), C54(H54), C55(H55), 
  C56(H56), C61(H61), C64(H64), C70(H70), C73(H73), C77(H77), C78(H78), 
 C79(H79), C80(H80), C81(H81), C83(H83), C84(H84), C85(H85), C86(H86), C87(H87), 
  C89(H89), C90(H90), C91(H91), C92(H92), C93(H93), C2S(H2S), C3S(H3S), C4S(H4S) 
3.b Idealised Me refined as rotating group: 
 C12(H12A,H12B,H12C), C15(H15A,H15B,H15C), C18(H18A,H18B,H18C), C21(H21A,H21B, 
 H21C), C24(H24A,H24B,H24C), C27(H27A,H27B,H27C), C36(H36A,H36B,H36C), C39(H39A, 
 H39B,H39C), C42(H42A,H42B,H42C), C45(H45A,H45B,H45C), C48(H48A,H48B,H48C), 
 C51(H51A,H51B,H51C), C60(H60A,H60B,H60C), C63(H63A,H63B,H63C), C66(H66A,H66B, 
 H66C), C69(H69A,H69B,H69C), C72(H72A,H72B,H72C), C75(H75A,H75B,H75C), C1S(H1SA, 
 H1SB,H1SC) 
;
_shelx_res_checksum              38465
_shelx_hkl_checksum              71673
_olex2_submission_special_instructions 'No special instructions were received'