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_7123753
_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         'C43 H71 Co Na O7 P3'
_chemical_formula_sum            'C43 H71 Co Na O7 P3'
_chemical_formula_weight         874.82
_chemical_name_systematic        P2PCoCONaDME3
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-10-30
_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                 97.3840(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1659(4)
_cell_length_b                   16.1007(5)
_cell_length_c                   26.6135(8)
_cell_measurement_reflns_used    9102
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.44
_cell_volume                     4744.9(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      200.0
_diffrn_measured_fraction_theta_full 0.998
_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  0.0209
_diffrn_reflns_av_unetI/netI     0.0100
_diffrn_reflns_Laue_measured_fraction_full 0.998
_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       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            103826
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.438
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.516
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7028
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0933 before and 0.0458 after correction. The Ratio of minimum to maximum transmission is 0.9426. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_description       block
_exptl_crystal_F_000             1872
_refine_diff_density_max         0.332
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     575
_refine_ls_number_reflns         10881
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0268
_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^)+(0.0380P)^2^+1.7820P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0741
_refine_ls_wR_factor_ref         0.0759
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10157
_reflns_number_total             10881
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc04032c2.cif
_cod_data_source_block           full_CCDC1
_cod_database_code               7123753
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H10(0.035) H14(0.036) H22(0.041) H13(0.035) H7(0.04) H3(0.043)
 H29(0.038) H26(0.038) H11(0.04) H25(0.041) H24(0.052) H17(0.04) H12(0.041)
 H6(0.05) H5(0.054) H16A(0.07) H16B(0.07) H16C(0.07) H27A(0.069) H27B(0.069)
 H27C(0.069) H23(0.051) H4(0.055) H30A(0.07) H30B(0.07) H30C(0.07) H28A(0.084)
 H28B(0.084) H28C(0.084) H15A(0.079) H15B(0.079) H15C(0.079) H18A(0.072)
 H18B(0.072) H18C(0.072) H19A(0.074) H19B(0.074) H19C(0.074) H37A(0.081)
 H37B(0.081) H31A(0.095) H31B(0.095) H31C(0.095) H36A(0.098) H36B(0.098)
 H36C(0.098) H34A(0.069) H34B(0.069) H35A(0.089) H35B(0.089) H35C(0.089)
 H38A(0.096) H38B(0.096) H39A(0.14) H39B(0.14) H39C(0.14) H42A(0.1) H42B(0.1)
 H43A(0.198) H43B(0.198) H43C(0.198) H32A(0.162) H32B(0.162) H32C(0.162)
 H40A(0.12) H40B(0.12) H40C(0.12) H41A(0.069) H41B(0.069) H41C(0.093)
 H41D(0.093) H40D(0.134) H40E(0.134) H40F(0.134) H42C(0.072) H42D(0.072)
 H43D(0.121) H43E(0.121) H43F(0.121)
 Fixed X: H10(0.2526) H14(0.286) H22(0.7456) H13(0.6403) H7(0.6586) H3(0.921)
 H29(0.8062) H26(0.6265) H11(0.2914) H25(0.7929) H24(0.8698) H17(0.1891)
 H12(0.4856) H6(0.8048) H5(1.0096) H16A(0.4808) H16B(0.4228) H16C(0.5194)
 H27A(0.5192) H27B(0.4355) H27C(0.415) H23(0.8429) H4(1.066) H30A(0.8669)
 H30B(0.9596) H30C(0.9072) H28A(0.448) H28B(0.4451) H28C(0.556) H15A(0.3557)
 H15B(0.2836) H15C(0.2224) H18A(0.2485) H18B(0.159) H18C(0.3011) H19A(0.3104)
 H19B(0.1685) H19C(0.221) H37A(0.8635) H37B(0.9643) H31A(0.7055) H31B(0.8403)
 H31C(0.7316) H36A(0.7266) H36B(0.8217) H36C(0.7218) H34A(0.5578) H34B(0.5371)
 H35A(0.8446) H35B(0.7401) H35C(0.7629) H38A(1.0632) H38B(1.0544) H39A(0.9669)
 H39B(1.0582) H39C(1.077) H42A(0.7156) H42B(0.7801) H43A(0.674) H43B(0.7097)
 H43C(0.6034) H32A(0.445) H32B(0.4414) H32C(0.3416) H40A(1.0354) H40B(1.0391)
 H40C(1.0934) H41A(0.7337) H41B(0.841) H41C(0.9667) H41D(0.9112) H40D(1.0498)
 H40E(1.0067) H40F(1.0383) H42C(0.8849) H42D(0.7475) H43D(0.7803) H43E(0.6537)
 H43F(0.6705)
 Fixed Y: H10(0.5501) H14(0.5855) H22(0.8908) H13(0.513) H7(0.4944) H3(0.6478)
 H29(0.9404) H26(0.9664) H11(0.4412) H25(0.6035) H24(0.6749) H17(0.6925)
 H12(0.4222) H6(0.4028) H5(0.433) H16A(0.532) H16B(0.5388) H16C(0.6062)
 H27A(0.8688) H27B(0.9482) H27C(0.8652) H23(0.8183) H4(0.5549) H30A(0.7991)
 H30B(0.8718) H30C(0.813) H28A(0.9518) H28B(1.0255) H28C(1.0178) H15A(0.7226)
 H15B(0.6444) H15C(0.7024) H18A(0.8131) H18B(0.8377) H18C(0.8529) H19A(0.7552)
 H19B(0.7694) H19C(0.6772) H37A(0.6902) H37B(0.6231) H31A(0.9936) H31B(0.9723)
 H31C(0.9114) H36A(0.5774) H36B(0.5369) H36C(0.6004) H34A(0.7055) H34B(0.6231)
 H35A(0.6489) H35B(0.585) H35C(0.6661) H38A(0.7237) H38B(0.7537) H39A(0.9312)
 H39B(0.8937) H39C(0.8739) H42A(0.9064) H42B(0.993) H43A(0.9736) H43B(1.0413)
 H43C(0.9765) H32A(0.8504) H32B(0.9216) H32C(0.8497) H40A(0.7298) H40B(0.7791)
 H40C(0.8208) H41A(0.8456) H41B(0.8848) H41C(0.9221) H41D(0.9045) H40D(0.7723)
 H40E(0.8041) H40F(0.8697) H42C(0.9787) H42D(0.9902) H43D(1.0367) H43E(1.0339)
 H43F(0.9837)
 Fixed Z: H10(0.3009) H14(0.3915) H22(0.2288) H13(0.257) H7(0.3741) H3(0.3381)
 H29(0.3264) H26(0.2736) H11(0.2478) H25(0.2431) H24(0.178) H17(0.3373)
 H12(0.2256) H6(0.4116) H5(0.4125) H16A(0.4089) H16B(0.4607) H16C(0.4476)
 H27A(0.2201) H27B(0.2253) H27C(0.2561) H23(0.1702) H4(0.3753) H30A(0.3896)
 H30B(0.3807) H30C(0.3346) H28A(0.3409) H28B(0.3005) H28C(0.3447) H15A(0.4567)
 H15B(0.4747) H15C(0.4297) H18A(0.3853) H18B(0.3357) H18C(0.3376) H19A(0.2575)
 H19B(0.2574) H19C(0.2552) H37A(0.4522) H37B(0.4728) H31A(0.3903) H31B(0.415)
 H31C(0.4237) H36A(0.5377) H36B(0.5047) H36C(0.479) H34A(0.6512) H34B(0.6173)
 H35A(0.6294) H35B(0.6389) H35C(0.6735) H38A(0.5274) H38B(0.4696) H39A(0.5241)
 H39B(0.4883) H39C(0.5478) H42A(0.6396) H42B(0.6323) H43A(0.5073) H43B(0.5507)
 H43C(0.556) H32A(0.5153) H32B(0.557) H32C(0.5517) H40A(0.6271) H40B(0.6795)
 H40C(0.6328) H41A(0.6505) H41B(0.6898) H41C(0.6309) H41D(0.6831) H40D(0.6399)
 H40E(0.6916) H40F(0.6501) H42C(0.6276) H42D(0.638) H43D(0.5413) H43E(0.5634)
 H43F(0.5129)
;
_shelx_res_checksum              20388
_olex2_submission_special_instructions 'No special instructions were received'