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_4086750
_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
'C18 H31 Cl Co N4, 1.472(C H4 O), Cl, 0.529(H2 O)'
_chemical_formula_sum            'C19.47 H37.95 Cl2 Co N4 O2'
_chemical_formula_weight         490.03
_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     direct
_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                   10.6094(4)
_cell_length_b                   17.5808(6)
_cell_length_c                   12.7464(4)
_cell_measurement_reflns_used    16295
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.938
_cell_measurement_theta_min      2.254
_cell_volume                     2360.80(14)
_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 0.998
_diffrn_measured_fraction_theta_max 0.850
_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  0.0380
_diffrn_reflns_av_unetI/netI     0.0584
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.850
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16295
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.850
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.938
_diffrn_reflns_theta_min         2.254
_diffrn_source                   'fine focus X-ray tube'
_exptl_absorpt_coefficient_mu    0.972
_exptl_absorpt_correction_T_max  0.686
_exptl_absorpt_correction_T_min  0.521
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_description       needle
_exptl_crystal_F_000             1039.2
_exptl_crystal_size_max          0.900
_exptl_crystal_size_mid          0.480
_exptl_crystal_size_min          0.420
_refine_diff_density_max         0.498
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       0.0031(6)
_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   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         6375
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0392
_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^)+(0.0478P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0891
_refine_ls_wR_factor_ref         0.0992
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4343
_reflns_number_total             6375
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00657_si_002.cif
_cod_data_source_block           1a
_cod_depositor_comments
'Adding full bibliography for 4086750--4086755.cif.'
_cod_database_code               4086750
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.475
_shelx_estimated_absorpt_t_max   0.686
_shelx_res_checksum              70319
_shelx_hkl_checksum              45475