Synthesis and Crystal Structure of 1,3-Bis(5-chloro-3-methoxysalicylideneamino)-2-propanol Trihydrate
MIKURIYA, Masahiro; KOYAMA, Yoshiki; MITSUHASHI, Ryoji; X-ray Structure Analysis Online 35 (2019) 33–; doi:10.2116/xraystruct.35.33

data_1551527
_publ_section_title
;
 Synthesis and Crystal Structure of
 1,3-Bis(5-chloro-3-methoxysalicylideneamino)-2-propanol Trihydrate
;
_journal_issue                   0
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              33
_journal_paper_doi               10.2116/xraystruct.35.33
_journal_volume                  35
_journal_year                    2019
_chemical_formula_sum            'C19 H26 Cl2 N2 O8'
_chemical_formula_weight         481.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 104.283(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.098(3)
_cell_length_b                   4.3275(8)
_cell_length_c                   14.572(3)
_cell_measurement_reflns_used    6637
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.499
_cell_measurement_theta_min      2.832
_cell_volume                     1106.0(4)
_computing_cell_refinement       'SAINT V8.35A (Bruker AXS Inc., 2015)'
_computing_data_collection       'APEX3 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.35A (Bruker AXS Inc., 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'XT, VERSION 2014/4'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6637
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.832
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.342
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.935
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_description       needle
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.338
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         2540
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0903
_refine_ls_R_factor_gt           0.0734
_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^)+(0.1205P)^2^+1.1291P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2011
_refine_ls_wR_factor_ref         0.2140
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1984
_reflns_number_total             2540
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            35_33_1.txt
_cod_data_source_block           H3cmsapm_0ma
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-Scan' changed to
'multi-scan' according to
/home/andrius/struct/COD-crude-data/automatic-downloads/current/J-STAGE/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 5642 2017-10-24 12:04:52Z antanas 
;
_cod_original_cell_volume        1106.0(3)
_cod_database_code               1551527
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.935
_shelx_estimated_absorpt_t_max   0.983
_shelx_res_checksum              61341
_shelx_hkl_checksum              47983