Unsymmetric Mononuclear and Bridged Dinuclear CoIII(cyclam) Acetylides
Cook, Timothy D.; Fanwick, Phillip E.; Ren, Tong; Organometallics 33 (2014) 4621–; doi:10.1021/om401231j

data_4082836
_publ_section_title
;
 Unsymmetric Mononuclear and Bridged Dinuclear CoIII(cyclam) Acetylides
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4621
_journal_paper_doi               10.1021/om401231j
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C20 H29 Co1 N4,Cl1,2(C1 H4 O1)'
_chemical_formula_sum            'C44 H74 Cl2 Co2 N8 O4'
_chemical_formula_weight         967.87
_chemical_name_systematic
;
 ?
;
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 98.070(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.9897(10)
_cell_length_b                   11.1484(8)
_cell_length_c                   18.9252(17)
_cell_measurement_reflns_used    25408
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      56.918
_cell_measurement_theta_min      4.615
_cell_volume                     2504.6(4)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'Crystal Clear(Rigaku 2001)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_publication_material  'local programs'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'DIRDIF/PATTY (Burskens, et. al,. 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.732
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku Rapid II'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.110
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 0.732
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25408
_diffrn_reflns_point_group_measured_fraction_full 0.732
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         56.918
_diffrn_reflns_theta_min         4.615
_diffrn_source                   'microfocus source'
_exptl_absorpt_coefficient_mu    6.539
_exptl_absorpt_correction_T_max  0.456
_exptl_absorpt_correction_T_min  0.127
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_description       needle
_exptl_crystal_F_000             1028
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.619
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         3325
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0993
_refine_ls_R_factor_gt           0.0850
_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^)+(0.1622P)^2^+2.3369P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2318
_refine_ls_wR_factor_ref         0.2499
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2644
_reflns_number_total             3325
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om401231j_si_002.cif
_cod_data_source_block           TC189A
_cod_database_code               4082836
_shelx_estimated_absorpt_t_min   0.303
_shelx_estimated_absorpt_t_max   0.484
_shelxl_version_number           2013-3
_shelx_res_checksum              67438
_shelx_hkl_checksum              58775
_shelx_fab_checksum              92403