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

data_4515078
_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            'C98 H58 F18 N6'
_chemical_formula_weight         1661.50
_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   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 99.8990(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.1182(19)
_cell_length_b                   15.1767(17)
_cell_length_c                   30.383(3)
_cell_measurement_reflns_used    9201
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.36
_cell_measurement_theta_min      2.83
_cell_volume                     7775.9(14)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/5 Bruker-AXS, Madison WI'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.39
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_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  0.0618
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            163422
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.930
_diffrn_reflns_theta_max         31.419
_diffrn_reflns_theta_min         1.543
_diffrn_source
;
Advanced Light Source, beamline 12.2.1
;
_exptl_absorpt_coefficient_mu    0.119
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.862
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 - Bruker AXS, Madison WI'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_description       lath
_exptl_crystal_F_000             3400
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.753
_refine_diff_density_min         -0.624
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1135
_refine_ls_number_reflns         23766
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0630
_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^)+(0.0931P)^2^+4.4239P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1758
_refine_ls_wR_factor_ref         0.1895
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17362
_reflns_number_total             23766
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao9b00275_si_002.cif
_cod_data_source_block           CF3azuliBenz_a
_cod_original_cell_volume        7775.8(15)
_cod_database_code               4515078
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.970
_shelx_estimated_absorpt_t_max   0.999
_shelx_res_checksum              33086
_shelx_hkl_checksum              16513