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_4132585
_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         'C51 H75 Co K N O'
_chemical_formula_sum            'C51 H75 Co K N O'
_chemical_formula_weight         816.15
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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                90
_cell_angle_beta                 108.693(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1895(6)
_cell_length_b                   42.067(3)
_cell_length_c                   10.8206(6)
_cell_measurement_reflns_used    1712
_cell_measurement_temperature    100
_cell_measurement_theta_max      21.91
_cell_measurement_theta_min      2.21
_cell_volume                     4824.7(5)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0723
_diffrn_reflns_av_unetI/netI     0.1293
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            15464
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.406
_diffrn_reflns_theta_max         24.406
_diffrn_reflns_theta_min         1.921
_diffrn_source                   'rotating anode'
_diffrn_source_type              fine-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.476
_exptl_absorpt_correction_T_max  0.6462
_exptl_absorpt_correction_T_min  0.5491
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0712 before and 0.0439 after correction. The Ratio of minimum to maximum transmission is 0.8497. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'dull dark orange'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.124
_exptl_crystal_description       plate
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     519
_refine_ls_number_reflns         7905
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.1360
_refine_ls_R_factor_gt           0.0592
_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^)+(0.0522P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1083
_refine_ls_wR_factor_ref         0.1321
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4452
_reflns_number_total             7905
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b05019_si_002.cif
_cod_data_source_block           JFig1122
_cod_database_code               4132585
_publcif_datablock.id            {1b72817c-aac0-4034-92e5-39e7569f33dc}
_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:
 C10(H10), C18(H18), C13(H13), C24(H24), C34(H34), C29(H29)
2.b Secondary CH2 refined with riding coordinates:
 C47(H47A,H47B), C49(H49A,H49B)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C4(H4), C5(H5), C21(H21), C16(H16), C32(H32), C27(H27)
2.d Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C11(H11A,H11B,H11C), C46(H46A,H46B,H46C), C19(H19A,H19B,
 H19C), C38(H38A,H38B,H38C), C14(H14A,H14B,H14C), C12(H12A,H12B,H12C), C20(H20A,
 H20B,H20C), C42(H42A,H42B,H42C), C40(H40A,H40B,H40C), C35(H35A,H35B,H35C),
 C15(H15A,H15B,H15C), C36(H36A,H36B,H36C), C48(H48A,H48B,H48C), C31(H31A,H31B,
 H31C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C30(H30A,H30B,H30C), C50(H50A,
 H50B,H50C)
;
_shelx_res_checksum              6899
_shelx_hkl_checksum              74618
_olex2_submission_special_instructions 'No special instructions were received'