Structural and Thermodynamic Features of Three Stable Crystal Forms of Temazepam: A Sedative Drug
Jetti, Ram K. R.; Bhogala, Balakrishna R.; Gorantla, Asha R.; Karusula, Nageswara R.; Datta, Debashish; Crystal Growth & Design 11 (2011) 2039–; doi:10.1021/cg1015675

data_4500468
_publ_section_title
;
 Structural and Thermodynamic Features of Three Stable Crystal Forms of
 Temazepam: A Sedative Drug
;
_journal_issue                   6
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              2039
_journal_paper_doi               10.1021/cg1015675
_journal_volume                  11
_journal_year                    2011
_chemical_formula_moiety         C16H13ClN2O2
_chemical_formula_sum            'C16 H13 Cl N2 O2'
_chemical_formula_weight         300.73
_chemical_melting_point          411.5
_chemical_name_common            Temazepam
_chemical_name_systematic
; 
 7-Chloro-1,3-dihydro-3-hydroxy-1-methyl-5-phenyl-2H-1,4-benzodiazepin- 2-one
;
_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
_cell_angle_alpha                101.60(3)
_cell_angle_beta                 104.53(3)
_cell_angle_gamma                98.76(3)
_cell_formula_units_Z            4
_cell_length_a                   9.789(2)
_cell_length_b                   12.235(2)
_cell_length_c                   13.586(3)
_cell_measurement_reflns_used    4316
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      46.231
_cell_measurement_theta_min      3.567
_cell_volume                     1507.3(6)
_computing_cell_refinement       'Crystal structure'
_computing_data_collection       'Crystal clear 2.0'
_computing_data_reduction        'Crystal structure'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Rigaku Mercury375R/M CCD (XtaLAB mini)'
_diffrn_measurement_method       'phi and omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0922
_diffrn_reflns_av_sigmaI/netI    0.0700
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8565
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.59
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    0.259
_exptl_absorpt_correction_T_max  0.9696
_exptl_absorpt_correction_T_min  0.9501
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Blocks
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         6799
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0935
_refine_ls_R_factor_gt           0.0707
_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^)+(0.1178P)^2^+0.2276P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1932
_refine_ls_wR_factor_ref         0.2262
_reflns_number_gt                4901
_reflns_number_total             6799
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg1015675_si_002.cif
_cod_data_source_block           Form-VI
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1507.3(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4500468