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_4088069
_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         'C18 H31 Cl1 Co1 N4,Cl1,2(C1 H4 O1)'
_chemical_formula_sum            'C20 H39 Cl2 Co N4 O2'
_chemical_formula_weight         497.38
_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'
_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                 96.791(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6098(5)
_cell_length_b                   17.5811(6)
_cell_length_c                   12.7469(4)
_cell_measurement_reflns_used    16054
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.271
_cell_measurement_theta_min      1.983
_cell_volume                     2361.02(16)
_computing_cell_refinement       'HKL3000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'Crystal Clear(Rigaku 2001)'
_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      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
Data were collected on a Rigaku Rapid which has a quarter 
chi circle and a 200 degree curved image plate at a fixed 
distance of 127.4mm.  Strategy was optimized using the 
CrystalClear software.  The completeness is the best 
that can be obtained with this geometry. The missing data are not 
cusp data but mostly high angle data.
Also the use of HKL3000/SCALEPACK lowers the number 
of observed data as inconsistent equivalents are removed 
from the data set and not included in the collected total.
;
_diffrn_measurement_device_type  'Rigaku Rapid II'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.033
_diffrn_reflns_av_unetI/netI     0.0482
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16054
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.271
_diffrn_reflns_theta_min         1.983
_diffrn_source                   'microfocus source'
_exptl_absorpt_coefficient_mu    0.976
_exptl_absorpt_correction_T_max  0.664
_exptl_absorpt_correction_T_min  0.310
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_description       needle
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.900
_exptl_crystal_size_mid          0.480
_exptl_crystal_size_min          0.420
_refine_diff_density_max         2.273
_refine_diff_density_min         -1.647
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         5792
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0886
_refine_ls_R_factor_gt           0.0639
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1228P)^2^+0.8096P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1825
_refine_ls_wR_factor_ref         0.1981
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4193
_reflns_number_total             5792
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00833_si_002.cif
_cod_data_source_block           SN137C
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4088069
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.474
_shelx_estimated_absorpt_t_max   0.685
_shelx_res_checksum              76506
_shelx_hkl_checksum              24939