Selective preparation of elusive and alternative single component polymorphic solid forms through multi-component crystallisation routes
Lynne H. Thomas; Craig Wales; Chick C. Wilson; Chem.Commun. 52 (2016) 7372–; doi:

data_7119164
_publ_section_title
;
 Selective preparation of elusive and alternative single component
 polymorphic solid forms through multi-component crystallisation routes
;
_journal_name_full               Chem.Commun.
_journal_page_first              7372
_journal_volume                  52
_journal_year                    2016
_chemical_formula_sum            'C46 H43 N9 O13 S3'
_chemical_formula_weight         1026.08
_chemical_name_systematic        'piroxicam methanol solvate'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-02-01 deposited with the CCDC.
2016-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                84.077(7)
_cell_angle_beta                 89.174(7)
_cell_angle_gamma                83.327(6)
_cell_formula_units_Z            2
_cell_length_a                   7.0374(19)
_cell_length_b                   12.917(4)
_cell_length_c                   25.467(8)
_cell_measurement_reflns_used    5509
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.18
_cell_measurement_theta_min      3.02
_cell_volume                     2287.0(12)
_computing_cell_refinement       'CrystalClear 1.4.0 (Rigaku, 2008)'
_computing_data_collection       'CrystalClear 1.4.0 (Rigaku, 2008)'
_computing_data_reduction        'CrystalClear 1.4.0 (Rigaku, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP Image Plate'
_diffrn_measurement_method       'Image plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.2357
_diffrn_reflns_av_sigmaI/netI    0.2334
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            14992
_diffrn_reflns_theta_full        20.82
_diffrn_reflns_theta_max         20.82
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    0.236
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.2351
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR, Rigaku 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1032
_refine_diff_density_max         1.498
_refine_diff_density_min         -1.383
_refine_diff_density_rms         0.192
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.440
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         4731
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.440
_refine_ls_R_factor_all          0.3371
_refine_ls_R_factor_gt           0.2271
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4776
_refine_ls_wR_factor_ref         0.5325
_reflns_number_gt                2059
_reflns_number_total             4731
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6cc01027j2.cif
_cod_data_source_block           shelxl_4
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7119164