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_4088677
_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 H76 Co N3 O3, 2(C2.48 H6), 0.05(C7 H8)'
_chemical_formula_sum            'C83.28 H88.37 Co N3 O3'
_chemical_formula_weight         1238.23
_chemical_melting_point          ?
_chemical_name_common            Co(Mes2NCC(H)NArMes2)(CO)3(CNArMes2)
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_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                   26.2209(13)
_cell_length_b                   18.8401(9)
_cell_length_c                   14.1228(7)
_cell_measurement_reflns_used    8362
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      25.42
_cell_measurement_theta_min      2.38
_cell_volume                     6976.7(6)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0381
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            28752
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.481
_diffrn_reflns_theta_min         1.553
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.297
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6245
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0501 before and 0.0438 after correction.
The Ratio of minimum to maximum transmission is 0.8380.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'Lusterous Yellow'
_exptl_crystal_colour_lustre     Lusterous
_exptl_crystal_colour_modifier   Yellow
_exptl_crystal_density_diffrn    1.179
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2640
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         6678
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0562P)^2^+4.0864P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1103
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5615
_reflns_number_total             6678
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00297_si_002.cif
_cod_data_source_block           jfig569_0ma
_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_database_code               4088677
_shelx_estimated_absorpt_t_max   0.943
_shelx_estimated_absorpt_t_min   0.916
_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. Restrained distances
 H6SC-C12S
 2.666 with sigma of 0.02
 H6SB-C12S
 2.684 with sigma of 0.02
 H6SA-H1SC
 2.27 with sigma of 0.02
3. Restrained planarity
 C6S, C7S, C8S, C9S, C10S, C11S, C12S
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C7S) = Uanis(C8S) = Uanis(C6S) = Uanis(C9S) = Uanis(C10S) = Uanis(C11S) =
Uanis(C12S) = Uanis(C52) = Uanis(C50) = Uanis(C49) = Uanis(C51)
5. Rigid body (RIGU) restrains
 C1S, C2S, C3S, C4S, C5S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C6S)=Sof(H6SA)=Sof(H6SB)=Sof(H6SC)=Sof(C9S)=Sof(H9S)=Sof(C10S)=Sof(H10S)=
 Sof(C11S)=Sof(H11S)=Sof(C12S)=Sof(H12S)=Sof(C7S)=Sof(C8S)=Sof(H8S)=0.5*(1-
 FVAR(2))
 Sof(C5S)=0.5*FVAR(2)
 Fixed Sof: C1S(0.5) H1SA(0.5) H1SB(0.5) H1SC(0.5) C2S(0.5) H2SA(0.5)
 H2SB(0.5) C3S(0.5) H3SA(0.5) H3SB(0.5) C4S(0.5) H4SA(0.5) H4SB(0.5) H5SA(0.5)
 H5SB(0.5) H5SC(0.5)
 Fixed X: C6S(0.584419)
 Fixed Y: C6S(0.25348)
 Fixed Z: C6S(-0.023992)
7.a Secondary CH2 refined with riding coordinates:
 C2S(H2SA,H2SB), C3S(H3SA,H3SB), C4S(H4SA,H4SB)
7.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C25(H25), C28(H28), C34(H34), C35(H35), C49(H49),
 C52(H52), C58(H58), C59(H59), C73(H73), C76(H76), C9S(H9S), C10S(H10S),
 C11S(H11S), C12S(H12S), C8S(H8S)
7.c Fitted hexagon refined as free rotating group:
 C9S(C10S,C11S,C12S,C7S,C8S)
7.d Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C27(H27A,H27B,H27C), C30(H30A,H30B,H30C), C48(H48A,H48B,
 H48C), C51(H51A,H51B,H51C), C54(H54A,H54B,H54C), C72(H72A,H72B,H72C), C75(H75A,
 H75B,H75C), C78(H78A,H78B,H78C), C1S(H1SA,H1SB,H1SC), C5S(H5SA,H5SB,H5SC),
 C6S(H6SA,H6SB,H6SC)
;
_shelx_res_checksum              4459
_shelx_hkl_checksum              99583
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'