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_4088668
_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 H104 Co N4, 2(C6 H12)'
_chemical_formula_sum            'C112 H128 Co N4'
_chemical_formula_weight         1589.11
_chemical_melting_point          ?
_chemical_name_common            Co(H)(CNArMes2)4
_chemical_name_systematic
hydridotetrakis(2,6-dimesitylphenylioscyanide)cobalt
_space_group_crystal_system      tetragonal
_space_group_IT_number           122
_space_group_name_Hall           'I -4 2bw'
_space_group_name_H-M_alt        'I -4 2 d'
_atom_sites_solution_hydrogens   mixed
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.4917(8)
_cell_length_b                   27.4917(8)
_cell_length_c                   11.7280(5)
_cell_measurement_reflns_used    3862
_cell_measurement_temperature    100
_cell_measurement_theta_max      56.79
_cell_measurement_theta_min      3.22
_cell_volume                     8863.9(5)
_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
_diffrn_measured_fraction_theta_full 0.996
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0479
_diffrn_reflns_av_unetI/netI     0.0469
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            18327
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        58.656
_diffrn_reflns_theta_max         58.656
_diffrn_reflns_theta_min         3.215
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.906
_exptl_absorpt_correction_T_max  0.7515
_exptl_absorpt_correction_T_min  0.6459
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS-2008/1 (Bruker,2008) was used for absorption correction. 
wR2(int) was 0.1013 before and 0.0641 after correction. 
The Ratio of minimum to maximum transmission is 0.8595. 
The \l/2 correction factor is 0.0015. 
;
_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    1.191
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3420
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.166
_refine_diff_density_min         -0.173
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details
; 
 Flack x determined using 1069 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.006(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         3122
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0369
_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^)+(0.0584P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0923
_refine_ls_wR_factor_ref         0.0956
_reflns_Friedel_coverage         0.795
_reflns_Friedel_fraction_full    0.981
_reflns_Friedel_fraction_max     0.981
_reflns_number_gt                2782
_reflns_number_total             3122
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00297_si_002.cif
_cod_data_source_block           jfig497
_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_colour_primary' value 'Orange' was changed
to 'orange' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

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        8863.9(6)
_cod_database_code               4088668
_shelx_estimated_absorpt_t_max   0.832
_shelx_estimated_absorpt_t_min   0.449
_olex2_refinement_description
; 
1. Fixed Uiso 
 At 1.2 times of: 
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups 
 At 1.5 times of: 
  All C(H,H,H) groups 
2. Restrained distances 
 Co1-H 
 1.5 with sigma of 0.02 
3. Rigid body (RIGU) restrains 
 C2T, C2S, C3S, C1S 
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 
4. Others 
 Sof(H1SC)=Sof(H1SD)=Sof(H3SD)=Sof(H3SC)=Sof(C2T)=Sof(H2TA)=Sof(H2TB)=1-FVAR(1) 
 Sof(H1SA)=Sof(H1SB)=Sof(C2S)=Sof(H2SA)=Sof(H2SB)=Sof(H3SB)=Sof(H3SA)=FVAR(1) 
5.a Secondary CH2 refined with riding coordinates: 
 C1S(H1SA,H1SB), C1S(H1SC,H1SD), C2S(H2SA,H2SB), C3S(H3SB,H3SA), C3S(H3SD, 
 H3SC), C2T(H2TA,H2TB) 
5.b Aromatic/amide H refined with riding coordinates: 
 C4(H4), C5(H5), C6(H6), C11(H11), C14(H14), C20(H20), C23(H23) 
5.c Idealised Me refined as rotating group: 
 C10(H10A,H10B,H10C), C13(H13A,H13B,H13C), C16(H16A,H16B,H16C), C19(H19A,H19B, 
 H19C), C22(H22A,H22B,H22C), C25(H25A,H25B,H25C) 
;
_shelx_res_checksum              35361
_shelx_hkl_checksum              8785
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'