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_4132584
_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         'C47 H64 Co I2 N'
_chemical_formula_sum            'C47 H64 Co I2 N'
_chemical_formula_weight         955.72
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2016-07-25
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.07.25 svn.r3318 for OlexSys, GUI svn.r5204)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.0483(13)
_cell_length_b                   14.0290(9)
_cell_length_c                   27.3737(18)
_cell_measurement_reflns_used    7529
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.31
_cell_measurement_theta_min      2.26
_cell_volume                     8851.1(10)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2013.6-2 (Bruker, 2013)'
_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, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker APEX CCD'
_diffrn_detector_area_resol_mean 8.0
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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_reflns_av_R_equivalents  0.0693
_diffrn_reflns_av_unetI/netI     0.0677
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            56422
_diffrn_reflns_point_group_measured_fraction_full 0.939
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.381
_diffrn_reflns_theta_min         1.451
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.814
_exptl_absorpt_correction_T_max  0.0916
_exptl_absorpt_correction_T_min  0.0650
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1080 before and 0.0665 after correction.
The Ratio of minimum to maximum transmission is 0.7096.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'dull dark brown'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_description       needle
_exptl_crystal_F_000             3888
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.980
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details
;
 Flack x determined using 4538 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.348(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     929
_refine_ls_number_reflns         15163
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0296P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0818
_refine_ls_wR_factor_ref         0.0897
_reflns_Friedel_coverage         0.834
_reflns_Friedel_fraction_full    0.875
_reflns_Friedel_fraction_max     0.868
_reflns_number_gt                12276
_reflns_number_total             15163
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b05019_si_002.cif
_cod_data_source_block           jfig1371_b
_cod_database_code               4132584
_publcif_datablock.id            {1065b071-05f6-4bef-907f-e95c921a87e7}
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C80) = Uanis(C78) = Uanis(C82)
Uanis(C88) = Uanis(C86) = Uanis(C90)
3.a Ternary CH refined with riding coordinates:
 C47(H47), C35(H35), C30(H30), C57(H57), C72(H72), C62(H62), C25(H25),
 C67(H67), C52(H52), C15(H15), C10(H10), C20(H20)
3.b Aromatic/amide H refined with riding coordinates:
 C43(H43), C6(H6), C33(H33), C50(H50), C70(H70), C55(H55), C42(H42), C28(H28),
 C65(H65), C5(H5), C13(H13), C41(H41), C4(H4), C18(H18)
3.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C88(H88A,H88B,H88C), C94(H94A,H94B,H94C), C48(H48A,H48B,
 H48C), C27(H27A,H27B,H27C), C74(H74A,H74B,H74C), C86(H86A,H86B,H86C), C26(H26A,
 H26B,H26C), C78(H78A,H78B,H78C), C84(H84A,H84B,H84C), C63(H63A,H63B,H63C),
 C32(H32A,H32B,H32C), C37(H37A,H37B,H37C), C82(H82A,H82B,H82C), C49(H49A,H49B,
 H49C), C21(H21A,H21B,H21C), C36(H36A,H36B,H36C), C92(H92A,H92B,H92C), C64(H64A,
 H64B,H64C), C31(H31A,H31B,H31C), C80(H80A,H80B,H80C), C69(H69A,H69B,H69C),
 C12(H12A,H12B,H12C), C17(H17A,H17B,H17C), C68(H68A,H68B,H68C), C59(H59A,H59B,
 H59C), C73(H73A,H73B,H73C), C76(H76A,H76B,H76C), C53(H53A,H53B,H53C), C58(H58A,
 H58B,H58C), C22(H22A,H22B,H22C), C90(H90A,H90B,H90C), C54(H54A,H54B,H54C),
 C11(H11A,H11B,H11C)
;
_shelx_res_checksum              90956
_shelx_hkl_checksum              45893
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'