Synthesis and Characterization of Free-Base, Copper, and Nickel Isocorroles
Giuseppe Pomarico; Xiao Xiao; Sara Nardis; Roberto Paolesse; Frank R. Fronczek; Kevin M. Smith; Yuanyuan Fang; Zhongping Ou; Karl M. Kadish; Inorganic Chemistry 49 (2010) 5766–5774; doi:10.1021/ic100730j

data_4315855
_publ_section_title
;
 Synthesis and Characterization of Free-Base, Copper, and Nickel
 Isocorroles
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5766
_journal_page_last               5774
_journal_paper_doi               10.1021/ic100730j
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C41 H32 Cu N4 O, C H Cl3 '
_chemical_formula_sum            'C42 H33 Cl3 Cu N4 O'
_chemical_formula_weight         779.61
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                79.320(6)
_cell_angle_beta                 85.260(6)
_cell_angle_gamma                70.830(9)
_cell_formula_units_Z            2
_cell_length_a                   7.6453(8)
_cell_length_b                   11.2802(10)
_cell_length_c                   21.863(2)
_cell_measurement_reflns_used    4097
_cell_measurement_temperature    90.0(5)
_cell_measurement_theta_max      68.2
_cell_measurement_theta_min      4.1
_cell_volume                     1749.6(3)
_computing_cell_refinement       'Bruker (2006) Apex-II '
_computing_data_collection       'Bruker (2006) Apex-II'
_computing_data_reduction        'Bruker (2006) Apex-II '
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'Bruker SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90.0(5)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.039
_diffrn_reflns_av_sigmaI/netI    0.0462
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            15861
_diffrn_reflns_theta_full        66.6
_diffrn_reflns_theta_max         68.7
_diffrn_reflns_theta_min         2.0
_exptl_absorpt_coefficient_mu    3.313
_exptl_absorpt_correction_T_max  0.937
_exptl_absorpt_correction_T_min  0.417
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2004)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             802
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
The 117 electrons per cell removed by SQUEEZE correspond closely to
two disordered chloroform molecules per unit cell. So the compound is
formulated as the mono-chloroform solvate, and the solvent is included
in the formula, formula weight, density, absoption coefficient, etc.
;
_refine_diff_density_max         0.44
_refine_diff_density_min         -0.39
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         6194
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0643P)^2^+0.6862P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1279
_refine_ls_wR_factor_ref         0.1341
_reflns_number_gt                4817
_reflns_number_total             6194
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic100730j_si_002.cif
_cod_data_source_block           5GP
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4315855