Synthesis and Molecular Structure of a Copper Octaiodocorrole.
Thomassen, Ivar K.; McCormick, Laura J.; Ghosh, Abhik; ACS omega 3 (2018) 5106–5110; doi:10.1021/acsomega.8b00616

data_4515971
_publ_section_title
;
 Synthesis and Molecular Structure of a Copper Octaiodocorrole.
;
_journal_issue                   5
_journal_name_full               'ACS omega'
_journal_page_first              5106
_journal_page_last               5110
_journal_paper_doi               10.1021/acsomega.8b00616
_journal_volume                  3
_journal_year                    2018
_chemical_formula_sum            'C64 H28.36 Cl8 Cu I7.64 N7'
_chemical_formula_weight         2211.86
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                111.769(2)
_cell_angle_beta                 91.652(2)
_cell_angle_gamma                90.047(2)
_cell_formula_units_Z            2
_cell_length_a                   13.9951(7)
_cell_length_b                   14.2730(8)
_cell_length_c                   17.8450(10)
_cell_measurement_reflns_used    9765
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.86
_cell_measurement_theta_min      2.18
_cell_volume                     3308.7(3)
_computing_cell_refinement       'SAINT V8.38A Bruker-AXS, Madison WI'
_computing_data_collection       'Bruker APEX3 Bruker-AXS, Madison WI'
_computing_data_reduction        'SAINT V8.38A Bruker-AXS, Madison WI'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.39
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 with PHOTON II detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_reflns_av_R_equivalents  0.0570
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            126292
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.930
_diffrn_reflns_theta_max         31.899
_diffrn_reflns_theta_min         1.493
_diffrn_source
;
Advanced Light Source, beamline 12.2.1
;
_exptl_absorpt_coefficient_mu    4.510
_exptl_absorpt_correction_T_max  0.956
_exptl_absorpt_correction_T_min  0.888
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 - Bruker AXS, Madison WI'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.220
_exptl_crystal_description       lath
_exptl_crystal_F_000             2062
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.911
_refine_diff_density_min         -1.270
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     803
_refine_ls_number_reflns         21097
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0399
_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^)+13.5244P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0741
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16457
_reflns_number_total             21097
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao8b00616_si_001.cif
_cod_data_source_block           CuI8pCNPN_a
_cod_database_code               4515971
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.714
_shelx_estimated_absorpt_t_max   0.956
_shelx_res_checksum              5866
_shelx_hkl_checksum              50334