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_4132582
_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         'C55 H82.75 Co K2 N O2'
_chemical_formula_sum            'C55 H83 Co K2 N O2'
_chemical_formula_weight         927.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 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                90
_cell_angle_beta                 121.309(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   46.323(2)
_cell_length_b                   12.1188(5)
_cell_length_c                   24.6506(10)
_cell_measurement_reflns_used    5901
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.038
_cell_measurement_theta_min      2.41
_cell_volume                     11823.2(9)
_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 0.998
_diffrn_measured_fraction_theta_max 0.993
_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  0.0678
_diffrn_reflns_av_unetI/netI     0.0706
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -55
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            39483
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.347
_diffrn_reflns_theta_min         1.029
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.465
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6621
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.0645 before and 0.0494 after correction. The Ratio of minimum to maximum transmission is 0.8885. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'dull blackish orange'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   blackish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.042
_exptl_crystal_description       plate
_exptl_crystal_F_000             4008
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     619
_refine_ls_number_reflns         10751
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0489
_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^)+(0.0498P)^2^+6.8829P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0999
_refine_ls_wR_factor_ref         0.1122
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7412
_reflns_number_total             10751
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b05019_si_002.cif
_cod_data_source_block           JFig1117
_cod_database_code               4132582
_publcif_datablock.id            {687c3c80-7894-4fbd-86af-24b0c0f9022d}
_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. Restrained distances
 C50-O2
 1.412 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C36A) = Uanis(C36)
4. Others
 Sof(C36A)=Sof(H36D)=Sof(H36E)=Sof(H36F)=1-FVAR(1)
 Sof(H34)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C10(H10), C15(H15), C25(H25), C34(H34), C29(H29), C20(H20)
5.b Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C54(H54A,H54B), C49(H49A,H49B), C50(H50A,H50B), C53(H53A,H53B)
5.c Aromatic/amide H refined with riding coordinates:
 C18(H18), C5(H5), C2AA(H2AA), C32(H32), C6(H6), C13(H13), C37(H37)
5.d Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C26(H26A,H26B,
 H26C), C43(H43A,H43B,H43C), C30(H30A,H30B,H30C), C45(H45A,H45B,H45C), C16(H16A,
 H16B,H16C), C21(H21A,H21B,H21C), C31(H31A,H31B,H31C), C35(H35A,H35B,H35C),
 C56(H56A,H56B,H56C), C17(H17A,H17B,H17C), C47(H47A,H47B,H47C), C48(H48A,H48B,
 H48C), C36(H36A,H36B,H36C), C36A(H36D,H36E,H36F)
;
_shelx_res_checksum              13260
_shelx_hkl_checksum              81242
_shelx_fab_checksum              13501
_olex2_submission_special_instructions 'No special instructions were received'