Azulicorrole
Larsen, Simon; McCormick-McPherson, Laura J.; Teat, Simon J.; Ghosh, Abhik; ACS Omega 4 (2019) 6737–; doi:10.1021/acsomega.9b00275

data_4515079
_publ_section_title
;
 Azulicorrole
;
_journal_issue                   4
_journal_name_full               'ACS Omega'
_journal_page_first              6737
_journal_paper_doi               10.1021/acsomega.9b00275
_journal_volume                  4
_journal_year                    2019
_chemical_formula_sum            'C49.5 H27 Cu F9 N3'
_chemical_formula_weight         898.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'Dual space'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                90
_cell_angle_beta                 96.358(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.5930(12)
_cell_length_b                   18.0587(12)
_cell_length_c                   11.9975(8)
_cell_measurement_reflns_used    9818
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.1024
_cell_measurement_theta_min      2.3129
_cell_volume                     3788.2(4)
_computing_cell_refinement       'Bruker SAINT v8.38a'
_computing_data_collection       'Bruker APEX 3'
_computing_data_reduction        'Bruker SAINT v8.38a'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL & local programs'
_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 0.997
_diffrn_measurement_device_type  'Bruker D8 with PHOTONII detector'
_diffrn_measurement_method       '\w/\q shutterless scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            122388
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.930
_diffrn_reflns_theta_max         29.145
_diffrn_reflns_theta_min         2.313
_diffrn_source                   'Advanced Light Source beamline 12.2.1'
_exptl_absorpt_coefficient_mu    0.709
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_correction_T_min  0.847
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2016/2 Bruker AXS Madison WI USA'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_description       plate
_exptl_crystal_F_000             1820
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.498
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     624
_refine_ls_number_reflns         9430
_refine_ls_number_restraints     91
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0425
_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^)+(0.0518P)^2^+4.5579P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1080
_refine_ls_wR_factor_ref         0.1159
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8068
_reflns_number_total             9430
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao9b00275_si_003.cif
_cod_data_source_block           cu-azuli-tol_a
_cod_original_formula_sum        'C49.50 H27 Cu F9 N3'
_cod_database_code               4515079
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.933
_shelx_estimated_absorpt_t_max   0.972
_shelx_res_checksum              53280
_shelx_hkl_checksum              70640