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_7123752
_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         'C31 H42 Co O P3'
_chemical_formula_sum            'C31 H42 Co O P3'
_chemical_formula_weight         582.48
_chemical_name_systematic        P2PCoCOH
_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   mixed
_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                102.756(3)
_cell_angle_beta                 98.244(2)
_cell_angle_gamma                103.517(3)
_cell_formula_units_Z            2
_cell_length_a                   9.4357(4)
_cell_length_b                   9.6576(6)
_cell_length_c                   17.4658(8)
_cell_measurement_reflns_used    9708
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.83
_cell_volume                     1477.06(13)
_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      99.99
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0444
_diffrn_reflns_av_unetI/netI     0.0139
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            104914
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.504
_diffrn_reflns_theta_min         2.720
_exptl_absorpt_coefficient_mu    0.766
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6883
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1004 before and 0.0431 after correction. The Ratio of minimum to maximum transmission is 0.9231. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_description       plate
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.314
_exptl_crystal_size_min          0.184
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         6787
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0207
_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^)+(0.0233P)^2^+0.6764P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0530
_refine_ls_wR_factor_ref         0.0535
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6375
_reflns_number_total             6787
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc04032c2.cif
_cod_data_source_block           v18277
_cod_database_code               7123752
_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.a Ternary CH refined with riding coordinates:
 C14(H14), C26(H26), C29(H29), C17(H17)
2.b Aromatic/amide H refined with riding coordinates:
 C24(H24), C21(H21), C22(H22), C6(H6), C23(H23), C4(H4), C5(H5), C7(H7),
 C12(H12), C9(H9), C10(H10), C11(H11), C3(H3)
2.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C27(H27A,H27B,H27C), C31(H31A,H31B,
 H31C), C15(H15A,H15B,H15C), C19(H19A,H19B,H19C), C30(H30A,H30B,H30C), C28(H28A,
 H28B,H28C)
;
_shelx_res_checksum              70655
_olex2_submission_special_instructions 'No special instructions were received'