Crystal structures and phase transformation of two novel solvates of valnemulin hydrochloride
Ouyang, Jinbo; Na, Bing; Zhou, Limin; Xiao, Saijin; Xiong, Guoxuan; Jin, Tianxiang; CrystEngComm 20 (2018) 563–; doi:10.1039/C7CE01524K

data_7229756
_publ_section_title
;
 Crystal structures and phase transformation of two novel solvates of
 valnemulin hydrochloride
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              563
_journal_paper_doi               10.1039/C7CE01524K
_journal_volume                  20
_journal_year                    2018
_chemical_absolute_configuration unk
_chemical_formula_sum            'C33 H61 Cl N2 O7 S'
_chemical_formula_weight         665.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-10-20 deposited with the CCDC.
2017-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.34(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.4013(17)
_cell_length_b                   16.424(3)
_cell_length_c                   13.536(3)
_cell_measurement_reflns_used    18792
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      72.9
_cell_measurement_theta_min      1.99
_cell_volume                     1809.5(7)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'rigaku r-axis rapid'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_av_unetI/netI     0.0786
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18792
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.969
_diffrn_reflns_theta_min         1.987
_exptl_absorpt_coefficient_mu    0.209
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.959
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   crystalclear
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_description       block
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.218
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Flack x determined using 2038 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         8347
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0480
_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^)+(0.0360P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0832
_refine_ls_wR_factor_ref         0.0903
_reflns_Friedel_coverage         0.864
_reflns_Friedel_fraction_full    0.940
_reflns_Friedel_fraction_max     0.922
_reflns_number_gt                6563
_reflns_number_total             8347
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01524k1.cif
_cod_data_source_block           VHWES
_cod_depositor_comments
'Adding full bibliography for 7229756--7229757.cif.'
_cod_database_code               7229756
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.959
_shelx_estimated_absorpt_t_max   0.975
_shelx_res_checksum              570