Developmental considerations for ethanolates with regard to stability and physicochemical characterization of efonidipine hydrochloride ethanolate
Otsuka, M.; Maeno, Y.; Fukami, T.; Inoue, M.; Tagami, T.; Ozeki, T.; CrystEngComm 17 (2015) 7430–; doi:10.1039/C5CE00751H

data_1529455
_publ_section_title
;
 Developmental considerations for ethanolates with regard to stability and
 physicochemical characterization of efonidipine hydrochloride ethanolate
;
_journal_issue                   38
_journal_name_full               CrystEngComm
_journal_page_first              7430
_journal_paper_doi               10.1039/C5CE00751H
_journal_volume                  17
_journal_year                    2015
_chemical_formula_sum            'C36 H45 Cl N3 O8 P'
_chemical_formula_weight         714.17
_chemical_name_common            NZ-105
_chemical_name_systematic
; 
 efonidipine hydrochloride ethanolate
;
_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
;
2015-07-31 deposited with the CCDC.
2015-08-21 downloaded from the CCDC.
;
_cell_angle_alpha                87.156(5)
_cell_angle_beta                 78.155(5)
_cell_angle_gamma                64.918(4)
_cell_formula_units_Z            2
_cell_length_a                   11.4763(11)
_cell_length_b                   11.9281(12)
_cell_length_c                   15.1054(15)
_cell_measurement_reflns_used    9998
_cell_measurement_temperature    296
_cell_measurement_theta_max      64.75
_cell_measurement_theta_min      2.99
_cell_volume                     1831.3(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'HELIOS multilayer optics'
_diffrn_radiation_source         'TURBO X-RAY SOURCE'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_sigmaI/netI    0.0164
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            25692
_diffrn_reflns_theta_full        65.63
_diffrn_reflns_theta_max         65.63
_diffrn_reflns_theta_min         2.99
_exptl_absorpt_coefficient_mu    1.784
_exptl_absorpt_correction_T_max  0.8704
_exptl_absorpt_correction_T_min  0.7757
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS Sheldrick 1996'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.793
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         5958
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0433
_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^)+(0.1000P)^2^+0.6811P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1418
_refine_ls_wR_factor_ref         0.1533
_reflns_number_gt                5362
_reflns_number_total             5958
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce00751h2.cif
_cod_data_source_block           efonidipine_hydrochloride_ethanolate
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 1529454--1529455.cif.

The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'const' was replaced with the
value 'constr' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1529455