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_7123755
_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 H41 Co O P3, C16 H32 Na O8'
_chemical_formula_sum            'C47 H73 Co Na O9 P3'
_chemical_formula_weight         956.88
_chemical_name_systematic        P2PCoCONacrown
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-11-04
_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                 132.65
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.599(3)
_cell_length_b                   30.400(5)
_cell_length_c                   18.698(2)
_cell_measurement_reflns_used    9986
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.38
_cell_volume                     11538(3)
_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_detector                 'CMOS Area Detector'
_diffrn_detector_area_resol_mean 10.24
_diffrn_detector_type            'Bruker PHOTON 100 CMOS'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            182977
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.034
_diffrn_reflns_theta_min         2.379
_diffrn_source                   'I\mS HB micro-focus sealed tube'
_diffrn_source_current           1
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatech I\mS HB'
_diffrn_source_voltage           50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.432
_exptl_absorpt_correction_T_max  0.7287
_exptl_absorpt_correction_T_min  0.6826
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1635 before and 0.0864 after correction. The Ratio of minimum to maximum transmission is 0.9367. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.102
_exptl_crystal_description       block
_exptl_crystal_F_000             4080
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.993
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     714
_refine_ls_number_reflns         21603
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0592
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0594P)^2^+20.9722P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1435
_refine_ls_wR_factor_ref         0.1527
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16818
_reflns_number_total             21603
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc04032c2.cif
_cod_data_source_block           v18425
_cod_original_cell_volume        11539(3)
_cod_database_code               7123755
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.878
_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(O8B) = Uanis(O8A)
Uanis(C17A) = Uanis(C17B)
3. Rigid body (RIGU) restrains
 C19A, C19B, C17A, C17B, C18B, C18A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C19A)=Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(C15A)=Sof(H15A)=Sof(H15B)=
 Sof(H15C)=Sof(C14A)=Sof(H14A)=Sof(C16A)=Sof(H16A)=Sof(H16B)=Sof(H16C)=
 Sof(C18A)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C17A)=Sof(H17A)=1-FVAR(1)
 Sof(C17B)=Sof(H17B)=Sof(C18B)=Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(C19B)=
 Sof(H19D)=Sof(H19E)=Sof(H19F)=Sof(C14B)=Sof(H14B)=Sof(C15B)=Sof(H15D)=
 Sof(H15E)=Sof(H15F)=Sof(C16B)=Sof(H16D)=Sof(H16E)=Sof(H16F)=FVAR(1)
 Sof(O9B)=Sof(C45B)=Sof(H45C)=Sof(H45D)=Sof(C44B)=Sof(H44C)=Sof(H44D)=Sof(O8B)=
 Sof(C43B)=Sof(H43C)=Sof(H43D)=Sof(C42B)=Sof(H42C)=Sof(H42D)=Sof(O7B)=Sof(C41B)=
 Sof(H41C)=Sof(H41D)=Sof(C40B)=Sof(H40C)=Sof(H40D)=Sof(O6B)=Sof(C47B)=Sof(H47C)=
 Sof(H47D)=Sof(C46B)=Sof(H46C)=Sof(H46D)=1-FVAR(2)
 Sof(O8A)=Sof(O9A)=Sof(O7A)=Sof(O6A)=Sof(C44A)=Sof(H44A)=Sof(H44B)=Sof(C42A)=
 Sof(H42A)=Sof(H42B)=Sof(C43A)=Sof(H43A)=Sof(H43B)=Sof(C45A)=Sof(H45A)=
 Sof(H45B)=Sof(C46A)=Sof(H46A)=Sof(H46B)=Sof(C47A)=Sof(H47A)=Sof(H47B)=
 Sof(C41A)=Sof(H41A)=Sof(H41B)=Sof(C40A)=Sof(H40A)=Sof(H40B)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C29(H29), C26(H26), C17B(H17B), C14A(H14A), C17A(H17A), C14B(H14B)
5.b Secondary CH2 refined with riding coordinates:
 C39(H39A,H39B), C38(H38A,H38B), C36(H36A,H36B), C35(H35A,H35B), C32(H32A,
 H32B), C34(H34A,H34B), C37(H37A,H37B), C44A(H44A,H44B), C33(H33A,H33B),
 C42A(H42A,H42B), C43A(H43A,H43B), C45A(H45A,H45B), C46A(H46A,H46B), C47A(H47A,
 H47B), C41A(H41A,H41B), C40A(H40A,H40B), C45B(H45C,H45D), C44B(H44C,H44D),
 C43B(H43C,H43D), C42B(H42C,H42D), C41B(H41C,H41D), C40B(H40C,H40D), C47B(H47C,
 H47D), C46B(H46C,H46D)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C3(H3), C12(H12), C5(H5), C9(H9), C23(H23), C24(H24),
 C10(H10), C21(H21), C22(H22), C11(H11), C6(H6)
5.d Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C19A(H19A,H19B,
 H19C), C30(H30A,H30B,H30C), C15A(H15A,H15B,H15C), C16A(H16A,H16B,H16C),
 C18A(H18A,H18B,H18C), C18B(H18D,H18E,H18F), C19B(H19D,H19E,H19F), C15B(H15D,
 H15E,H15F), C16B(H16D,H16E,H16F)
;
_shelx_res_checksum              39232
_shelx_fab_checksum              34287
_olex2_submission_special_instructions 'No special instructions were received'