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_4088678
_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         'C50 H52 Co N2, C F3 O3 S'
_chemical_formula_sum            'C51 H52 Co F3 N2 O3 S'
_chemical_formula_weight         888.93
_chemical_melting_point          ?
_chemical_name_common            '[Co(HCHNArMes2)(CNArMes2)]OTf'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.8635(14)
_cell_length_b                   12.9587(11)
_cell_length_c                   23.5511(18)
_cell_measurement_reflns_used    2887
_cell_measurement_temperature    100
_cell_measurement_theta_max      23.10
_cell_measurement_theta_min      2.26
_cell_volume                     4536.2(7)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8.0
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.968
_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  0.0575
_diffrn_reflns_av_unetI/netI     0.1029
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13890
_diffrn_reflns_point_group_measured_fraction_full 0.810
_diffrn_reflns_point_group_measured_fraction_max 0.794
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.382
_diffrn_reflns_theta_min         1.729
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.481
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6157
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0762 before and 0.0592 after correction.
The Ratio of minimum to maximum transmission is 0.8262.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'orange orange'
_exptl_crystal_colour_lustre     orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1864
_exptl_crystal_recrystallization_method
'crystalized from a saturated solution at -35 C'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.448
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details
;
 Flack x determined using 1249 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.52(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         6617
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1354
_refine_ls_R_factor_gt           0.0719
_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^)+(0.0739P)^2^+6.4864P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1538
_refine_ls_wR_factor_ref         0.1838
_reflns_Friedel_coverage         0.597
_reflns_Friedel_fraction_full    0.631
_reflns_Friedel_fraction_max     0.610
_reflns_number_gt                4140
_reflns_number_total             6617
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00297_si_002.cif
_cod_data_source_block           jfig847
_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               4088678
_shelx_estimated_absorpt_t_max   0.953
_shelx_estimated_absorpt_t_min   0.910
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 S1SB-C1SB
 1.68 with sigma of 0.02
 S1SB-O2SB
 1.43 with sigma of 0.02
 S1SB-O1SB
 1.43 with sigma of 0.02
 S1SB-O3SB
 1.43 with sigma of 0.02
 O1SB-O3SB
 2.4 with sigma of 0.02
 O3SB-O2SB
 2.4 with sigma of 0.02
 O1SB-O2SB
 2.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C1A) \\sim Ueq, Uanis(C1B) \\sim Ueq, Uanis(C2A) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
Uanis(C2A) \\sim Ueq, Uanis(C1B) \\sim Ueq, Uanis(C1A) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
Uanis(C2A) = Uanis(C2B)
Uanis(C1B) = Uanis(C1A)
Uanis(C1S) = Uanis(S1S)
Uanis(S1SB) = Uanis(S1S)
Uanis(C1SB) = Uanis(C1S)
Uanis(F1SB) = Uanis(F2SB) = Uanis(F3SB) = Uanis(F3S) = Uanis(F1S)
Uanis(O3S) = Uanis(O1S) = Uanis(O2SB) = Uanis(O3SB) = Uanis(O1SB)
4. Others
 Sof(H2)=Sof(C1B)=Sof(H1B)=Sof(C2B)=Sof(Co1B)=1-FVAR(1)
 Sof(H1)=Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(Co1A)=FVAR(1)
 Sof(S1SB)=Sof(C1SB)=Sof(O1SB)=Sof(O2SB)=Sof(O3SB)=Sof(F3SB)=Sof(F2SB)=
 Sof(F1SB)=1-FVAR(2)
 Sof(C1S)=Sof(F1S)=Sof(F2S)=Sof(F3S)=Sof(O1S)=Sof(O2S)=Sof(O3S)=Sof(S1S)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C12(H12), C15(H15), C21(H21), C24(H24), C29(H29),
 C30(H30), C31(H31), C36(H36), C39(H39), C45(H45), C48(H48), N1(H1), N2(H2),
 C1A(H1A), C1B(H1B)
5.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C20(H20A,H20B,
 H20C), C23(H23A,H23B,H23C), C26(H26A,H26B,H26C), C35(H35A,H35B,H35C), C38(H38A,
 H38B,H38C), C41(H41A,H41B,H41C), C44(H44A,H44B,H44C), C47(H47A,H47B,H47C),
 C50(H50A,H50B,H50C)
;
_shelx_res_checksum              75009
_shelx_hkl_checksum              2683
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'