Mometasone furoate revisited, or how did the hydrate get in the bottle?
Müller, Peter; Acta Crystallographica Section C 71 (2015) –; doi:10.1107/S2053229615021476

data_2020298
_publ_section_title
;
 Mometasone furoate revisited, or how did the hydrate get in the bottle?
;
_journal_coeditor_code           OV3071
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229615021476
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C27 H30 Cl2 O6 , H2 O'
_chemical_formula_moiety         'C27 H30 Cl2 O6, H2 O'
_chemical_formula_sum            'C27 H32 Cl2 O7'
_chemical_formula_weight         539.42
_chemical_name_systematic
'9\a,21-Dichloro-11\b,17\a-dihydroxy-16\a-methyl-3,20-dioxodipregna-1,4-dien-17-yl furan-2-carboxylate monohydrate'
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     vecmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                73.617(5)
_cell_angle_beta                 85.522(6)
_cell_angle_gamma                69.492(5)
_cell_formula_units_Z            1
_cell_length_a                   7.2367(6)
_cell_length_b                   8.4193(6)
_cell_length_c                   11.7507(8)
_cell_measurement_reflns_used    2338
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.51
_cell_measurement_theta_min      3.92
_cell_volume                     643.17(9)
_computing_cell_refinement
;
SAINT (Bruker, 2014)
;
_computing_data_collection
;
APEX2 (Bruker, 2014)
;
_computing_data_reduction
;
SAINT (Bruker, 2014)
;
_computing_molecular_graphics
;
APEX2 (Bruker, 2014)
;
_computing_publication_material
;
APEX2 (Bruker, 2014)
;
_computing_structure_refinement
;
SHELXL2014/6 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0539
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9890
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         68.937
_diffrn_reflns_theta_min         3.922
_exptl_absorpt_coefficient_mu    2.652
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.5946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             284
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.008
_refine_diff_density_max         0.249
_refine_diff_density_min         -0.272
_refine_ls_abs_structure_details
;
Flack x parameter determined using 1106 quotients [(I^+^) - (I^-^)]/[(I^+^) +
(I^-^)]  (Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.033(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         3691
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0580P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0979
_refine_ls_wR_factor_ref         0.1002
_reflns_number_gt                3309
_reflns_number_total             3691
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ov3071sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        643.18(9)
_cod_database_code               2020298
_cod_database_fobs_code          2020298
_shelx_estimated_absorpt_t_min   0.879
_shelx_estimated_absorpt_t_max   0.979
_shelx_hkl_checksum              64701
_shelx_res_checksum              29415
_shelxl_version_number           2014/6