CoIII(cyclam) Oligoynyls: Monomeric Oligoynyl Complexes and Dimeric Complexes with an Oligoyn-diyl Bridge
Cook, Timothy D.; Natoli, Sean N.; Fanwick, Phillip E.; Ren, Tong; Organometallics  (2016) –; doi:10.1021/acs.organomet.6b00219

data_4086487
_publ_section_title
;
 CoIII(cyclam) Oligoynyls: Monomeric Oligoynyl Complexes and Dimeric
 Complexes with an Oligoyn-diyl Bridge
;
_journal_name_full               Organometallics
_journal_paper_doi               10.1021/acs.organomet.6b00219
_journal_year                    2016
_chemical_formula_moiety         'C26 H48 Cl2 Co2 N8, 4(C H4 O), 2(Cl)'
_chemical_formula_sum            'C30 H64 Cl4 Co2 N8 O4'
_chemical_formula_weight         860.55
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                63.560(3)
_cell_angle_beta                 73.330(3)
_cell_angle_gamma                75.371(3)
_cell_formula_units_Z            2
_cell_length_a                   10.7889(6)
_cell_length_b                   14.3914(9)
_cell_length_c                   15.0470(9)
_cell_measurement_reflns_used    20071
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.235
_cell_measurement_theta_min      1.992
_cell_volume                     1982.7(2)
_computing_cell_refinement       'HKL3000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'Nonius Collect (Nonius, 1998)'
_computing_data_reduction        'HKL3000 (Otwinowski & Minor, 1997)'
_computing_structure_refinement
;  
SHELXL-2014/7 (Sheldrick, 2014), 
SHELXLE Rev714 (H\"ubschle et al., 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Nonius Kappa CCD diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.038
_diffrn_reflns_av_unetI/netI     0.0588
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9560
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.235
_diffrn_reflns_theta_min         1.543
_diffrn_source                   'fine focus X-ray tube'
_exptl_absorpt_coefficient_mu    1.150
_exptl_absorpt_correction_T_max  0.795
_exptl_absorpt_correction_T_min  0.113
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_description       needle
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.377
_refine_diff_density_min         -0.624
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         9560
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.958
_refine_ls_R_factor_all          0.0711
_refine_ls_R_factor_gt           0.0475
_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^)+(0.0954P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1303
_refine_ls_wR_factor_ref         0.1413
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6942
_reflns_number_total             9560
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00219_si_003.cif
_cod_data_source_block           tc191b_MZ
_cod_database_code               4086487
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.545
_shelx_estimated_absorpt_t_max   0.803
_shelx_res_checksum              10528
_shelx_hkl_checksum              35864