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_4088070
_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         '2(C18 H30 Cl1 Co1 N4),2(Cl1),4(C1 H4 O1)'
_chemical_formula_sum            'C40 H76 Cl4 Co2 N8 O4'
_chemical_formula_weight         992.74
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 103.304(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.1438(10)
_cell_length_b                   9.9999(4)
_cell_length_c                   13.7463(5)
_cell_measurement_reflns_used    15442
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.332
_cell_measurement_theta_min      2.312
_cell_volume                     2560.9(2)
_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    'SHELXT (Sheldrick)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.973
_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  0.034
_diffrn_reflns_av_unetI/netI     0.0702
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            15442
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.332
_diffrn_reflns_theta_min         2.312
_diffrn_source                   'fine focus tube'
_exptl_absorpt_coefficient_mu    0.900
_exptl_absorpt_correction_T_max  0.914
_exptl_absorpt_correction_T_min  0.669
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_description       plate
_exptl_crystal_F_000             1052
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.411
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         6222
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.0887
_refine_ls_R_factor_gt           0.0435
_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^)+(0.0455P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.0997
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3819
_reflns_number_total             6222
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00833_si_002.cif
_cod_data_source_block           SN178C
_cod_original_cell_volume        2560.91(19)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4088070
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.687
_shelx_estimated_absorpt_t_max   0.915
_shelx_res_checksum              51769
_shelx_hkl_checksum              64420