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_4088674
_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         'C78 H85 Co N3 P, C2 H3 N'
_chemical_formula_sum            'C80 H88 Co N4 P'
_chemical_formula_weight         1195.44
_chemical_melting_point          ?
_chemical_name_common            CoH(PMe3)(CNArMes2)3
_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             2014-08-21
_audit_creation_method
; 
Olex2 1.2-beta 
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862) 
;
_cell_angle_alpha                98.851(5)
_cell_angle_beta                 91.101(5)
_cell_angle_gamma                110.393(4)
_cell_formula_units_Z            2
_cell_length_a                   13.363(2)
_cell_length_b                   15.442(2)
_cell_length_c                   17.940(3)
_cell_measurement_reflns_used    9959
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.019
_cell_measurement_theta_min      2.498
_cell_volume                     3418.0(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      100.0
_diffrn_detector_area_resol_mean 8.0
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.940
_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  0.0261
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            73916
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.210
_diffrn_reflns_theta_min         1.631
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.320
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS-2008/1 (Bruker,2008) was used for absorption correction. 
wR2(int) was 0.0803 before and 0.0358 after correction. 
The Ratio of minimum to maximum transmission is 0.9126. 
The \l/2 correction factor is 0.0015. 
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1276
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.442
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.051
_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     810
_refine_ls_number_reflns         19102
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0469P)^2^+1.7588P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0953
_refine_ls_wR_factor_ref         0.1034
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15771
_reflns_number_total             19102
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00297_si_002.cif
_cod_data_source_block           jfig636_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        3417.8(9)
_cod_database_code               4088674
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.969
_shelx_estimated_absorpt_t_min   0.910
_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, All C(H,H,H,H,H,H) groups 
2. Restrained distances 
 C1S-C2SB 
 1.5 with sigma of 0.02 
 N1S-C2SA 
 1.35 with sigma of 0.02 
3. Rigid bond restraints 
 C2SA, N1S 
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 
4. Uiso/Uaniso restraints and constraints 
Uanis(N1S) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 
5. Others 
 Sof(H1SA)=Sof(H1SB)=Sof(H1SC)=Sof(C2SA)=1-FVAR(1) 
 Sof(H1SD)=Sof(H1SE)=Sof(H1SF)=Sof(C2SB)=FVAR(1) 
6.a Aromatic/amide H refined with riding coordinates: 
 C9(H9), C10(H10), C11(H11), C16(H16), C20(H20), C26(H26), C29(H29), C34(H34), 
 C35(H35), C36(H36), C41(H41), C44(H44), C50(H50), C53(H53), C58(H58), C59(H59), 
  C60(H60), C65(H65), C68(H68), C74(H74), C77(H77) 
6.b Idealised Me refined with everything fixed: 
 C1S(H1SA,H1SB,H1SC), C1S(H1SD,H1SE,H1SF) 
6.c Idealised Me refined as rotating group: 
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C15(H15A,H15B,H15C), 
 C18(H18A,H18B,H18C), C22(H22A,H22B,H22C), C25(H25A,H25B,H25C), C28(H28A,H28B, 
 H28C), C31(H31A,H31B,H31C), C40(H40A,H40B,H40C), C43(H43A,H43B,H43C), C46(H46A, 
 H46B,H46C), C49(H49A,H49B,H49C), C52(H52A,H52B,H52C), C55(H55A,H55B,H55C), 
 C64(H64A,H64B,H64C), C67(H67A,H67B,H67C), C70(H70A,H70B,H70C), C73(H73A,H73B, 
 H73C), C76(H76A,H76B,H76C), C79(H79A,H79B,H79C) 
;
_shelx_res_checksum              93733
_shelx_hkl_checksum              13038
_olex2_submission_special_instructions 'No special instructions were received'