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_4132586
_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         'C54 H83 Co K N O Si, C5 H12'
_chemical_formula_sum            'C59 H86 Co K N O Si'
_chemical_formula_weight         951.40
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2017-04-01
_audit_creation_method
;
Olex2 1.2
(compiled Jan 19 2015 12:28:14 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2017-04-01 # Formatted by publCIF

;
_cell_angle_alpha                93.0540(10)
_cell_angle_beta                 104.8680(10)
_cell_angle_gamma                110.9260(10)
_cell_formula_units_Z            2
_cell_length_a                   12.4898(4)
_cell_length_b                   12.5227(4)
_cell_length_c                   20.6102(6)
_cell_measurement_reflns_used    9758
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.72
_cell_measurement_theta_min      2.18
_cell_volume                     2872.39(16)
_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, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_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 0.998
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II Ultra'
_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  0.0337
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            100317
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.943
_diffrn_reflns_theta_min         1.764
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.429
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7139
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0744 before and 0.0428 after correction.
The Ratio of minimum to maximum transmission is 0.9575.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'metallic light orange'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.100
_exptl_crystal_description       plate
_exptl_crystal_F_000             1030
_exptl_crystal_size_max          0.98
_exptl_crystal_size_mid          0.052
_exptl_crystal_size_min          0.019
_refine_diff_density_max         0.362
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     635
_refine_ls_number_reflns         13771
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0567P)^2^+0.9462P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1001
_refine_ls_wR_factor_ref         0.1080
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11252
_reflns_number_total             13771
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b05019_si_002.cif
_cod_data_source_block           JFig1199
_cod_database_code               4132586
_publcif_datablock.id            {d85fa9ab-89cd-403d-ac26-cbf861b2cda7}
_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. Uiso/Uaniso restraints and constraints
Uanis(C15A) = Uanis(C15B)
Uanis(C16A) = Uanis(C16B)
Uanis(C17A) = Uanis(C17B)
3. Others
 Sof(C16B)=Sof(H16D)=Sof(H16E)=Sof(H16F)=Sof(C15B)=Sof(H15B)=Sof(C17B)=
 Sof(H17D)=Sof(H17E)=Sof(H17F)=1-FVAR(1)
 Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C17A)=
 Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C25(H25), C35(H35), C10(H10), C30(H30), C20(H20), C15A(H15A), C15B(H15B)
4.b Secondary CH2 refined with riding coordinates:
 C53(H53A,H53B), C57(H57A,H57B), C52(H52A,H52B), C56(H56A,H56B), C58(H58A,H58B)
4.c Aromatic/amide H refined with riding coordinates:
 C33(H33), C4(H4), C6(H6), C28(H28), C5(H5), C18(H18), C13(H13)
4.d Idealised Me refined as rotating group:
 C48(H48A,H48B,H48C), C36(H36A,H36B,H36C), C50(H50A,H50B,H50C), C12(H12A,H12B,
 H12C), C3AA(H3AA,H3AB,H3AC), C49(H49A,H49B,H49C), C45(H45A,H45B,H45C),
 C31(H31A,H31B,H31C), C37(H37A,H37B,H37C), C26(H26A,H26B,H26C), C46(H46A,H46B,
 H46C), C32(H32A,H32B,H32C), C43(H43A,H43B,H43C), C47(H47A,H47B,H47C), C22(H22A,
 H22B,H22C), C27(H27A,H27B,H27C), C51(H51A,H51B,H51C), C21(H21A,H21B,H21C),
 C16A(H16A,H16B,H16C), C55(H55A,H55B,H55C), C59(H59A,H59B,H59C), C17A(H17A,H17B,
 H17C), C16B(H16D,H16E,H16F), C17B(H17D,H17E,H17F)
;
_shelx_res_checksum              73522
_shelx_hkl_checksum              91381
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'