Highly Reducible π-Extended Copper Corroles
Yadav, Pinky; Muniappan, Sankar; Ke, Xiangyi; Cong, Lei; Kadish, Karl M.; Dalton Trans.  (2017) –; doi:10.1039/C7DT01814B

data_7043621
_publ_section_title
;
 Highly Reducible \p-Extended Copper Corroles
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01814B
_journal_year                    2017
_chemical_formula_moiety         'C53 H31 Cu N4'
_chemical_formula_sum            'C53 H31 Cu N4'
_chemical_formula_weight         787.36
_chemical_name_common
'3,17-diphenylethynyl-5,10,15-tripenylcorrolatocopper(II) cation radical '
_chemical_name_systematic
'3,17-diphenylethynyl-5,10,15-tripenylcorrolatocopper(II) cation radical '
_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
_audit_block_doi                 10.5517/ccdc.csd.cc1nf5qz
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-07-11 deposited with the CCDC.
2017-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                117.549(3)
_cell_angle_beta                 109.011(3)
_cell_angle_gamma                97.510(3)
_cell_formula_units_Z            4
_cell_length_a                   16.7756(6)
_cell_length_b                   17.1514(5)
_cell_length_c                   18.3118(6)
_cell_measurement_reflns_used    17083
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.5800
_cell_measurement_theta_min      3.6240
_cell_volume                     4160.4(3)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.,'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.,'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.,'
_computing_molecular_graphics    Ortep3
_computing_publication_material  Shelx97
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 15.9948
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.861
_diffrn_measurement_device_type  'OXFORD DIFFRACTION SUPER NOVA'
_diffrn_measurement_method       \w/q-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Micro-Focus (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0716
_diffrn_reflns_av_unetI/netI     0.1240
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.861
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            54681
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.861
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.853
_diffrn_reflns_theta_min         2.906
_exptl_absorpt_coefficient_mu    0.566
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81458
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'DARK RED'
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1624
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Chloroform and Methanol'
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.140
_platon_squeeze_details
;
;
_refine_diff_density_max         1.794
_refine_diff_density_min         -1.538
_refine_diff_density_rms         0.197
_refine_ls_extinction_coef       0.0052(8)
_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   0.986
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1046
_refine_ls_number_reflns         26671
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.1118
_refine_ls_R_factor_gt           0.0770
_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^)+(0.1407P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2206
_refine_ls_wR_factor_ref         0.2607
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15766
_reflns_number_total             26671
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01814b2.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        4160.3(3)
_cod_database_code               7043621
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.881
_shelx_estimated_absorpt_t_max   0.925
_shelx_res_checksum              44899