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_7229757
_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            'C32 H59 Cl N2 O7 S'
_chemical_formula_weight         651.32
_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                 105.13(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.3555(17)
_cell_length_b                   16.471(3)
_cell_length_c                   13.319(3)
_cell_measurement_reflns_used    18142
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.91
_cell_measurement_theta_min      1.58
_cell_volume                     1769.5(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 0.997
_diffrn_measurement_device_type  'ragiku r-axis rapid'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_unetI/netI     0.0725
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18142
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.908
_diffrn_reflns_theta_min         1.584
_exptl_absorpt_coefficient_mu    0.213
_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    1.222
_exptl_crystal_description       block
_exptl_crystal_F_000             708
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.221
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details
;
'Flack H D (1983), Acta Cryst. A39, 876-881' 
;
_refine_ls_abs_structure_Flack   0.00(5)
_refine_ls_extinction_coef       0.033(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         7650
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0497P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0926
_refine_ls_wR_factor_ref         0.1005
_reflns_Friedel_coverage         0.934
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                5727
_reflns_number_total             7650
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01524k1.cif
_cod_data_source_block           VHWMS
_cod_depositor_comments
'Adding full bibliography for 7229756--7229757.cif.'
_cod_database_code               7229757
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.959
_shelx_estimated_absorpt_t_max   0.975
_shelx_res_checksum              56478