A Synthetic Approach to Cross-Conjugated Organometallic Complexes Based on geminal-Diethynylethene and CoIII(cyclam)
Natoli, Sean N.; Azbell, Tyler J.; Fanwick, Phillip E.; Zeller, Matthias; Ren, Tong; Organometallics 35 (2016) 3594–; doi:10.1021/acs.organomet.6b00657

data_4086754
_publ_section_title
;
 A Synthetic Approach to Cross-Conjugated Organometallic Complexes Based
 on geminal-Diethynylethene and CoIII(cyclam)
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              3594
_journal_paper_doi               10.1021/acs.organomet.6b00657
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety
'C32 H60 Co2 N10, 4(C F3 O3 S), 2.222(C2 H3 N)'
_chemical_formula_sum            'C40.44 H66.67 Co2 F12 N12.22 O12 S4'
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_space_group_crystal_system      triclinic
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_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'
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                66.088(3)
_cell_angle_beta                 81.683(3)
_cell_angle_gamma                87.985(3)
_cell_formula_units_Z            2
_cell_length_a                   13.1069(5)
_cell_length_b                   14.6343(5)
_cell_length_c                   17.3230(6)
_cell_measurement_reflns_used    68103
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.948
_cell_measurement_theta_min      4.562
_cell_volume                     3004.6(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      100(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'Nonius Kappa CCD diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1152
_diffrn_reflns_av_unetI/netI     0.0537
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            68103
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.948
_diffrn_reflns_theta_min         4.562
_diffrn_source                   'fine focus X-ray tube'
_exptl_absorpt_coefficient_mu    6.530
_exptl_absorpt_correction_T_max  0.623
_exptl_absorpt_correction_T_min  0.202
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_description       plate
_exptl_crystal_F_000             1433
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.748
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       0.00030(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1009
_refine_ls_number_reflns         11261
_refine_ls_number_restraints     740
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0925
_refine_ls_R_factor_gt           0.0719
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0669P)^2^+10.3304P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1708
_refine_ls_wR_factor_ref         0.1907
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8873
_reflns_number_total             11261
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00657_si_002.cif
_cod_data_source_block           4a
_cod_depositor_comments
'Adding full bibliography for 4086750--4086755.cif.'
_cod_database_code               4086754
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.370
_shelx_estimated_absorpt_t_max   0.623
_shelx_res_checksum              27340
_shelx_hkl_checksum              43217