Cobalt(III) Bridged by gem-DEE: Facile Access to a New Type of Cross-Conjugated Organometallics
Natoli, Sean N.; Cook, Timothy D.; Abraham, Tara R.; Kiernicki, John J.; Fanwick, Phillip E.; Ren, Tong; Organometallics 34 (2015) 5207–; doi:10.1021/acs.organomet.5b00833

data_4088068
_publ_section_title
;
 Cobalt(III) Bridged by gem-DEE: Facile Access to a New Type of
 Cross-Conjugated Organometallics
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              5207
_journal_paper_doi               10.1021/acs.organomet.5b00833
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C28 H54 Cl2 Co2 N8,2(Cl),3.5(C H4 O)'
_chemical_formula_sum            'C31.5 H68 Cl4 Co2 N8 O3.5'
_chemical_formula_weight         874.59
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                88.2800(10)
_cell_angle_beta                 77.0850(10)
_cell_angle_gamma                87.8280(10)
_cell_formula_units_Z            4
_cell_length_a                   14.1272(3)
_cell_length_b                   15.6818(4)
_cell_length_c                   19.7114(5)
_cell_measurement_reflns_used    43033
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.878
_cell_measurement_theta_min      1.617
_cell_volume                     4252.29(18)
_computing_cell_refinement       'HKL3000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'Nonius Collect (Nonius, 1998)'
_computing_data_reduction        'HKL3000 (Otwinowski & Minor, 1997)'
_computing_publication_material  'local programs'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'DIRDIF/PATTY (Burskens, et. al,. 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.035
_diffrn_reflns_av_unetI/netI     0.0546
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            43033
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.878
_diffrn_reflns_theta_min         1.617
_diffrn_source                   'fine focus tube'
_exptl_absorpt_coefficient_mu    1.073
_exptl_absorpt_correction_T_max  0.725
_exptl_absorpt_correction_T_min  0.078
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_description       plate
_exptl_crystal_F_000             1852
_exptl_crystal_size_max          0.660
_exptl_crystal_size_mid          0.540
_exptl_crystal_size_min          0.300
_refine_diff_density_max         1.823
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     895
_refine_ls_number_reflns         20006
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0786
_refine_ls_R_factor_gt           0.0543
_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^)+(0.0851P)^2^+2.0044P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1390
_refine_ls_wR_factor_ref         0.1506
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14555
_reflns_number_total             20006
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00833_si_002.cif
_cod_data_source_block           SN291
_cod_depositor_comments
;

2020-07-06
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C63 H136 Cl8 Co4 N16 O7'
_cod_original_formula_weight         1749.19
_cod_original_formula_moiety         '2(C28 H54 Cl2 Co2 N8),4(Cl1),7(C1 H4 O1)'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        4252.30(18)
_cod_database_code               4088068
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.538
_shelx_estimated_absorpt_t_max   0.739
_shelx_res_checksum              71277
_shelx_hkl_checksum              70830
_shelx_fab_checksum              65227