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_7123750
_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         'C30.96 H41 Br Co O0.96 P3, 1.5(C7 H8)'
_chemical_formula_sum            'C41.47 H53 Br Co O0.96 P3'
_chemical_formula_weight         798.61
_chemical_name_systematic        P2PCoBrCO
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                90
_cell_angle_beta                 101.797(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9453(6)
_cell_length_b                   14.9644(8)
_cell_length_c                   23.9133(15)
_cell_measurement_reflns_used    9683
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.36
_cell_volume                     3834.0(4)
_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 0.995
_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  0.0677
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            85776
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.137
_diffrn_reflns_theta_min         2.209
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.646
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6880
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0578 before and 0.0526 after correction. The Ratio of minimum to maximum transmission is 0.9227. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_description       Block
_exptl_crystal_F_000             1666
_exptl_crystal_size_max          0.141
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.092
_refine_diff_density_max         0.886
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         8438
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0313
_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^)+(0.0370P)^2^+2.4876P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0745
_refine_ls_wR_factor_ref         0.0771
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7232
_reflns_number_total             8438
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc04032c2.cif
_cod_data_source_block           mkt
_cod_database_code               7123750
_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(Br1B)=1-FVAR(1)
 Sof(Br1A)=Sof(O1)=Sof(C1)=FVAR(1)
 Fixed Sof: C40A(0.5) C42A(0.5) H42A(0.5) C44A(0.5) H44A(0.5) C43A(0.5)
 H43A(0.5) C39A(0.5) H39A(0.5) H39B(0.5) H39C(0.5) C41A(0.5) H41A(0.5)
 C45A(0.5) H45A(0.5)
3.a Ternary CH refined with riding coordinates:
 C26(H26), C20(H20), C29(H29), C23(H23)
3.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C15(H15), C16(H16), C17(H17), C7(H7), C3(H3), C9(H9), C4(H4),
 C6(H6), C12(H12), C11(H11), C10(H10), C5(H5), C38(H38), C37(H37), C34(H34),
 C35(H35), C36(H36), C42A(H42A), C44A(H44A), C43A(H43A), C41A(H41A), C45A(H45A)
3.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C28(H28A,H28B,H28C), C31(H31A,H31B,H31C), C30(H30A,H30B,
 H30C), C22(H22A,H22B,H22C), C27(H27A,H27B,H27C), C24(H24A,H24B,H24C), C25(H25A,
 H25B,H25C), C32(H32A,H32B,H32C), C39A(H39A,H39B,H39C)
;
_shelx_res_checksum              16439
_olex2_submission_special_instructions 'No special instructions were received'