O-Functionalization of a Cobalt Carbonyl Generates a Terminal Cobalt Carbyne
Deegan, Meaghan M.; Peters, Jonas C.; Chemical Communications  (2019) –; doi:10.1039/C9CC04032C

data_7123751
_publ_section_title
;
 O-Functionalization of a Cobalt Carbonyl Generates a Terminal Cobalt
 Carbyne
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC04032C
_journal_year                    2019
_chemical_formula_moiety         '1(C30.98 H41 Br0.02 Co O0.98 P3)'
_chemical_formula_sum            'C30.98 H41 Br0.02 Co O0.98 P3'
_chemical_formula_weight         582.51
_chemical_name_systematic        P2PCoCO
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-10-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-05-24 deposited with the CCDC.    2019-07-01 downloaded from the CCDC.
;
_cell_angle_alpha                109.036(7)
_cell_angle_beta                 92.528(7)
_cell_angle_gamma                90.859(8)
_cell_formula_units_Z            4
_cell_length_a                   10.843(2)
_cell_length_b                   16.079(3)
_cell_length_c                   17.991(3)
_cell_measurement_reflns_used    9456
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.33
_cell_volume                     2960.8(9)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0662
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            163632
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.509
_diffrn_reflns_theta_min         2.333
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.791
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6971
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0931 before and 0.0620 after correction. The Ratio of minimum to maximum transmission is 0.9350. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_description       block
_exptl_crystal_F_000             1230
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.221
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     715
_refine_ls_number_reflns         13550
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0248
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0342P)^2^+0.9748P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0663
_refine_ls_wR_factor_ref         0.0678
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11895
_reflns_number_total             13550
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc04032c2.cif
_cod_data_source_block           v18215_mmd
_cod_original_cell_volume        2960.7(10)
_cod_database_code               7123751
_shelx_shelxl_version_number     2014/7
_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. Others
 Sof(C60B)=Sof(H60B)=Sof(C61B)=Sof(H61D)=Sof(H61E)=Sof(H61F)=Sof(C62B)=
 Sof(H62D)=Sof(H62E)=Sof(H62F)=1-FVAR(1)
 Sof(C60A)=Sof(H60A)=Sof(C61A)=Sof(H61A)=Sof(H61B)=Sof(H61C)=Sof(C62A)=
 Sof(H62A)=Sof(H62B)=Sof(H62C)=FVAR(1)
 Sof(Br3)=1-FVAR(2)
 Sof(O2)=Sof(C32)=FVAR(2)
 Sof(Br1)=1-FVAR(3)
 Sof(O1)=Sof(C1)=FVAR(3)
3.a Ternary CH refined with riding coordinates:
 C29(H29), C17(H17), C26(H26), C14(H14), C45(H45), C48(H48), C57(H57),
 C60A(H60A), C60B(H60B)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C3(H3), C37(H37), C34(H34), C4(H4), C24(H24), C38(H38), C23(H23),
 C6(H6), C5(H5), C55(H55), C35(H35), C36(H36), C54(H54), C53(H53), C22(H22),
 C25(H25), C56(H56), C13(H13), C44(H44), C41(H41), C12(H12), C43(H43), C10(H10),
  C11(H11), C42(H42)
3.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C18(H18A,H18B,
 H18C), C31(H31A,H31B,H31C), C16(H16A,H16B,H16C), C46(H46A,H46B,H46C), C19(H19A,
 H19B,H19C), C49(H49A,H49B,H49C), C47(H47A,H47B,H47C), C58(H58A,H58B,H58C),
 C59(H59A,H59B,H59C), C15(H15A,H15B,H15C), C50(H50A,H50B,H50C), C61A(H61A,H61B,
 H61C), C62A(H62A,H62B,H62C), C61B(H61D,H61E,H61F), C62B(H62D,H62E,H62F)
;
_shelx_res_checksum              25709
_olex2_submission_special_instructions 'No special instructions were received'