Multicomponent Adducts of Pyridoxine: An Evaluation of the Formation of Eutectics and Molecular Salts
Ganduri, Ramesh; Cherukuvada, Suryanarayan; Guru Row, Tayur N.; Crystal Growth & Design 15 (2015) 3474–; doi:10.1021/acs.cgd.5b00546

data_4513560
_publ_section_title
;
 Multicomponent Adducts of Pyridoxine: An Evaluation of the Formation of
 Eutectics and Molecular Salts
;
_journal_issue                   7
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              3474
_journal_paper_doi               10.1021/acs.cgd.5b00546
_journal_volume                  15
_journal_year                    2015
_chemical_formula_moiety         'C8 H12 N O3, C7 H5 O3'
_chemical_formula_sum            'C15 H17 N O6'
_chemical_formula_weight         307.29
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-06-02
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 95.223(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.2676(15)
_cell_length_b                   6.8912(7)
_cell_length_c                   26.705(3)
_cell_measurement_reflns_used    5861
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      27.4360
_cell_measurement_theta_min      2.6810
_cell_volume                     2798.0(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0419
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega -101.00  -34.00   1.0000   21.0500
omega____ theta____ kappa____ phi______ frames
    -      -21.1163 -179.0000 -120.0000 67

  2 omega  -97.00   45.00   1.0000   21.0500
omega____ theta____ kappa____ phi______ frames
    -      -21.1163  -19.0000   90.0000 142

  3 omega  -53.00   52.00   1.0000   21.0500
omega____ theta____ kappa____ phi______ frames
    -      -21.1163   37.0000  -60.0000 105

  4 omega  -94.00   12.00   1.0000   21.0500
omega____ theta____ kappa____ phi______ frames
    -      -21.1163  -77.0000   30.0000 106

  5 omega   34.00  108.00   1.0000   21.0500
omega____ theta____ kappa____ phi______ frames
    -       25.4913 -179.0000 -150.0000 74

  6 omega    2.00   70.00   1.0000   21.0500
omega____ theta____ kappa____ phi______ frames
    -       25.4913   57.0000 -120.0000 68

  7 omega    2.00   96.00   1.0000   21.0500
omega____ theta____ kappa____ phi______ frames
    -       25.4913   57.0000  -30.0000 94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Nova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0340807000
_diffrn_orient_matrix_UB_12      0.0670185000
_diffrn_orient_matrix_UB_13      -0.0072450000
_diffrn_orient_matrix_UB_21      -0.0113454000
_diffrn_orient_matrix_UB_22      0.0036067000
_diffrn_orient_matrix_UB_23      0.0251898000
_diffrn_orient_matrix_UB_31      0.0296879000
_diffrn_orient_matrix_UB_32      0.0780449000
_diffrn_orient_matrix_UB_33      0.0050626000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0673
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            15977
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         2.679
_diffrn_source                   'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.114
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71138
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_description       plate
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.329
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         3203
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0590P)^2^+1.8456P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1201
_refine_ls_wR_factor_ref         0.1293
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2621
_reflns_number_total             3203
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            PN-PHBA.cif
_cod_data_source_block           PN-PHBA
_cod_database_code               4513560
_chemical_oxdiff_formula         'C15 H17 O6 N1'
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O6-H6
 0.992 with sigma of 0.001
 O3-H3
 0.992 with sigma of 0.001
 O2-H2
 0.97 with sigma of 0.001
 O1-H1
 0.97 with sigma of 0.001
 N1-H1A
 1.036 with sigma of 0.001
3.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B)
3.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C11(H11), C12(H12), C14(H14), C15(H15)
3.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'