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_4086488
_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         'C28 H48 Cl2 Co2 N8, 5(C H4 O), 2(Cl)'
_chemical_formula_sum            'C33 H68 Cl4 Co2 N8 O5'
_chemical_formula_weight         916.61
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                96.647(18)
_cell_angle_beta                 91.394(17)
_cell_angle_gamma                108.290(19)
_cell_formula_units_Z            2
_cell_length_a                   9.844(3)
_cell_length_b                   15.481(4)
_cell_length_c                   15.963(4)
_cell_measurement_reflns_used    51189
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      54.238
_cell_measurement_theta_min      2.793
_cell_volume                     2289.5(11)
_computing_cell_refinement       'HKL3000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'Crystal Clear (Rigaku 2001)'
_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      200(2)
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type
'Rigaku Rapid II curved image plate diffractometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'laterally graded multilayer (Goebel) mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.192
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.941
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            51189
_diffrn_reflns_point_group_measured_fraction_full 0.941
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.973
_diffrn_reflns_theta_min         4.383
_diffrn_source                   'microfocus X-ray tube'
_exptl_absorpt_coefficient_mu    8.182
_exptl_absorpt_correction_T_max  0.566
_exptl_absorpt_correction_T_min  0.143
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_description       plate
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.270
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         7823
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1484
_refine_ls_R_factor_gt           0.1084
_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^)+(0.1710P)^2^+10.4844P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2906
_refine_ls_wR_factor_ref         0.3340
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5243
_reflns_number_total             7823
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00219_si_003.cif
_cod_data_source_block           tc253b_MZ
_cod_original_cell_volume        2289.7(11)
_cod_database_code               4086488
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.291
_shelx_estimated_absorpt_t_max   0.736
_shelx_res_checksum              38564
_shelx_hkl_checksum              2699