Urochrome Pigment in Uric Acid Crystals
Hall, Victoria M.; Cox, Kristin A.; Sours, Ryan E.; Swift, Jennifer A.; Chemistry of Materials 28 (2016) 3862–; doi:10.1021/acs.chemmater.6b00977

data_4003238
_publ_section_title
;
 Urochrome Pigment in Uric Acid Crystals
;
_journal_issue                   11
_journal_name_full               'Chemistry of Materials'
_journal_page_first              3862
_journal_paper_doi               10.1021/acs.chemmater.6b00977
_journal_volume                  28
_journal_year                    2016
_chemical_formula_moiety         'C17 H13 N2, H O4 S, C2 H4 O2'
_chemical_formula_sum            'C19 H18 N2 O6 S'
_chemical_formula_weight         402.41
_chemical_name_common            'Urorosein Sulfate Acetate'
_chemical_name_systematic        3H-indol-1-ium-3-ylmethylene-3H-indol-1-ium
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.1106(17)
_cell_length_b                   7.3879(6)
_cell_length_c                   24.510(2)
_cell_measurement_reflns_used    57637
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.173
_cell_measurement_theta_min      5.237
_cell_volume                     3641.6(5)
_computing_cell_refinement       'SAINT v. 8.27B, Bruker-AXS'
_computing_data_collection       'APEX 2, Bruker-AXS'
_computing_data_reduction        'SAINT v. 8.27B, Bruker-AXS'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-Version 2013/1, G. Sheldrick'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            'Bruker APEXII'
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details      '0.5 degree frames measured 1.0 seconds each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_monochromator  'silicon 1 1 1 and 3 1 1'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.1928
_diffrn_reflns_av_unetI/netI     0.0825
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            53006
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        14.974
_diffrn_reflns_theta_max         14.974
_diffrn_reflns_theta_min         1.131
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.034
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8046
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2-12/1, G. Sheldrick'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_description       needle
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.005
_exptl_transmission_factor_max   1.0000
_exptl_transmission_factor_min   0.8046
_refine_diff_density_max         0.232
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         3657
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0965
_refine_ls_R_factor_gt           0.0479
_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^)+(0.0364P)^2^+1.7359P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.1088
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2400
_reflns_number_total             3657
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm6b00977_si_001.cif
_cod_data_source_block           Urorosein
_cod_original_cell_volume        3641.5(5)
_cod_database_code               4003238
_shelxl_version_number           2014/7
_shelx_estimated_absorpt_t_min   0.993
_shelx_estimated_absorpt_t_max   1.000
_shelx_res_checksum              35380
_shelx_hkl_checksum              26038