A Highly-Reduced Cobalt Terminal Carbyne: Divergent Metal- and α-Carbon-Centered Reactivity.
Mokhtarzadeh, Charles C.; Moore, Curtis E.; Rheingold, Arnold L.; Figueroa, Joshua S.; Journal of the American Chemical Society 140 (2018) 8100–8104; doi:10.1021/jacs.8b05019

data_4132583
_publ_section_title
;
 A Highly-Reduced Cobalt Terminal Carbyne: Divergent Metal- and
 \a-Carbon-Centered Reactivity.
;
_journal_issue                   26
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8100
_journal_page_last               8104
_journal_paper_doi               10.1021/jacs.8b05019
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C65 H85 Co K N O'
_chemical_formula_sum            'C65 H85 Co K N O'
_chemical_formula_weight         994.36
_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             2017-01-19
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_cell_angle_alpha                82.679(3)
_cell_angle_beta                 86.994(3)
_cell_angle_gamma                81.566(3)
_cell_formula_units_Z            2
_cell_length_a                   11.4478(6)
_cell_length_b                   12.1071(7)
_cell_length_c                   21.3849(12)
_cell_measurement_reflns_used    9971
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.38
_cell_measurement_theta_min      2.41
_cell_volume                     2906.3(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2014.11-0 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker X8 APEX II'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0954
_diffrn_reflns_av_unetI/netI     0.1120
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            46582
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.446
_diffrn_reflns_theta_min         1.860
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.407
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.2504
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.1843 before and 0.1039 after correction. The Ratio of minimum to maximum transmission is 0.3358. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'dull dark red'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_description       plate
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.049
_exptl_crystal_size_min          0.033
_refine_diff_density_max         2.234
_refine_diff_density_min         -1.369
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     645
_refine_ls_number_reflns         14496
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1134
_refine_ls_R_factor_gt           0.0904
_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^)+(0.1401P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2228
_refine_ls_wR_factor_ref         0.2386
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10092
_reflns_number_total             14496
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b05019_si_002.cif
_cod_data_source_block           JFig1208
_cod_database_code               4132583
_publcif_datablock.id            {3a65d904-0547-4e4b-a005-84456b89a141}
_shelx_shelxl_version_number     2014/7
_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.a Ternary CH refined with riding coordinates:
 C37(H37), C27(H27), C17(H17), C12(H12), C22(H22), C32(H32)
2.b Secondary CH2 refined with riding coordinates:
 C62(H62A,H62B), C64(H64A,H64B)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C7(H7), C20(H20), C15(H15), C41(H41), C30(H30), C35(H35),
 C47(H47), C51(H51), C45(H45), C50(H50), C42(H42), C49(H49), C48(H48), C44(H44),
  C43(H43)
2.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C29(H29A,H29B,H29C), C39(H39A,H39B,H39C), C28(H28A,H28B,
 H28C), C59(H59A,H59B,H59C), C57(H57A,H57B,H57C), C60(H60A,H60B,H60C), C18(H18A,
 H18B,H18C), C38(H38A,H38B,H38C), C61(H61A,H61B,H61C), C14(H14A,H14B,H14C),
 C58(H58A,H58B,H58C), C33(H33A,H33B,H33C), C13(H13A,H13B,H13C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C34(H34A,H34B,H34C), C63(H63A,H63B,H63C), C65(H65A,
 H65B,H65C)
;
_shelx_res_checksum              5615
_shelx_hkl_checksum              97566
_shelx_fab_checksum              28231
_olex2_submission_special_instructions 'No special instructions were received'