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_4086751
_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         'C19 H31 Co N5, F6 P, 0.756(C H4 O)'
_chemical_formula_sum            'C19.76 H34.02 Co F6 N5 O0.76 P'
_chemical_formula_weight         557.61
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 102.310(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9073(10)
_cell_length_b                   17.4468(11)
_cell_length_c                   12.4980(8)
_cell_measurement_reflns_used    15599
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      72.032
_cell_measurement_theta_min      5.070
_cell_volume                     2536.7(3)
_computing_cell_refinement       'HKL3000 (Otwinowski & Minor, 1997)'
_computing_data_collection
;
CrystalClear-SM Expert 2.1 b32 (Rigaku, 2014)
;
_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 0.940
_diffrn_measured_fraction_theta_max 0.904
_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  0.0729
_diffrn_reflns_av_unetI/netI     0.0726
_diffrn_reflns_Laue_measured_fraction_full 0.940
_diffrn_reflns_Laue_measured_fraction_max 0.904
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15599
_diffrn_reflns_point_group_measured_fraction_full 0.940
_diffrn_reflns_point_group_measured_fraction_max 0.904
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.032
_diffrn_reflns_theta_min         5.070
_diffrn_source                   'microfocus X-ray tube'
_exptl_absorpt_coefficient_mu    6.491
_exptl_absorpt_correction_T_max  0.563
_exptl_absorpt_correction_T_min  0.314
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_description       needle
_exptl_crystal_F_000             1158.4
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       0.00292(19)
_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   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         4511
_refine_ls_number_restraints     231
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0642
_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^)+(0.0145P)^2^+7.6437P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1436
_refine_ls_wR_factor_ref         0.1586
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3605
_reflns_number_total             4511
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00657_si_002.cif
_cod_data_source_block           2a
_cod_depositor_comments
'Adding full bibliography for 4086750--4086755.cif.'
_cod_database_code               4086751
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.305
_shelx_estimated_absorpt_t_max   0.563
_shelx_res_checksum              36299
_shelx_hkl_checksum              18874