Exploring charge density analysis in crystals at high pressure: data collection, data analysis and advanced modelling
Casati, Nicola; Genoni, Alessandro; Meyer, Benjamin; Krawczuk, Anna; Macchi, Piero; Acta Crystallographica Section B 73 (2017) 584–597; doi:10.1107/S2052520617008356

data_2108144
_publ_section_title
;
 Exploring charge density analysis in crystals at high pressure: data
 collection, data analysis and advanced modelling
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              584
_journal_page_last               597
_journal_paper_doi               10.1107/S2052520617008356
_journal_volume                  73
_journal_year                    2017
_chemical_formula_sum            'C16 H10 O2'
_chemical_formula_weight         234.24
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.780(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8423(5)
_cell_length_b                   12.2033(16)
_cell_length_c                   9.1817(12)
_cell_measurement_reflns_used    5136
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11.18
_cell_measurement_theta_min      1.54
_cell_volume                     989.59(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_pressure         1800000
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.689
_diffrn_measured_fraction_theta_max 0.689
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.3100
_diffrn_reflns_av_R_equivalents  0.0683
_diffrn_reflns_av_sigmaI/netI    0.0787
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5136
_diffrn_reflns_theta_full        11.18
_diffrn_reflns_theta_max         11.18
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    0.065
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.13308
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.44b (release 16-11-2010 CrysAlis171 .NET)
(compiled Nov 16 2010,21:40:38)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         1394
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1033
_refine_ls_R_factor_gt           0.0691
_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^)+(0.1484P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1865
_refine_ls_wR_factor_ref         0.2239
_reflns_number_gt                992
_reflns_number_total             1394
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            lc5086sup3.cif
_cod_data_source_block           BCA_1p80_GPa
_cod_database_code               2108144