Optimizing the morphology of calcium d-pantothenate by controlling phase transformation processes
Han, Dandan; Du, Shichao; Wu, Songgu; Ouyang, Ruiling; Gong, Junbo; CrystEngComm 23 (2021) 2162–2173; doi:10.1039/D0CE01803A

data_7242240
_publ_section_title
;
 Optimizing the morphology of calcium d-pantothenate by controlling phase
 transformation processes
;
_journal_issue                   10
_journal_name_full               CrystEngComm
_journal_page_first              2162
_journal_page_last               2173
_journal_paper_doi               10.1039/D0CE01803A
_journal_volume                  23
_journal_year                    2021
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C20 H40 Ca N2 O12, 2(C H4 O), H2 O'
_chemical_formula_sum            'C22 H50 Ca N2 O15'
_chemical_formula_weight         622.72
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-12-01
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2020-12-01 deposited with the CCDC.	2021-02-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.428(3)
_cell_length_b                   13.933(3)
_cell_length_c                   18.288(4)
_cell_measurement_reflns_used    30411
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.484
_cell_measurement_theta_min      3.128
_cell_volume                     3166.7(12)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'rigaku r-axis rapid'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0927
_diffrn_reflns_av_unetI/netI     0.1853
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            30411
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.128
_exptl_absorpt_coefficient_mu    0.265
_exptl_absorpt_correction_T_max  0.9615
_exptl_absorpt_correction_T_min  0.9369
_exptl_crystal_colour            'whiteish white'
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.548
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Flack x determined using 1322 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.05(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         7216
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1205
_refine_ls_R_factor_gt           0.0777
_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^)+(0.0922P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1636
_refine_ls_wR_factor_ref         0.1847
_reflns_Friedel_coverage         0.792
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                4650
_reflns_number_total             7216
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01803a2.cif
_cod_data_source_block           b
_cod_depositor_comments          'Adding full bibliography for 7242240.cif.'
_cod_database_code               7242240
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.937
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O4-H4
 0.9 with sigma of 0.02
 H8B-C8
 0.96 with sigma of 0.02
 H8C-C8
 0.96 with sigma of 0.02
 HW1A-O1
 2.2 with sigma of 0.02
3.a Free rotating group:
 OW1(HW1A,HW1B)
3.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C22(H22A,H22B,H22C), C21(H21A,H21B,H21C), C20(H20A,H20B,
 H20C), C19(H19A,H19B,H19C)
3.c Idealised tetrahedral OH refined as rotating group:
 O13(H13), O14(H14A)
;
_shelx_res_checksum              27089
_shelx_hkl_checksum              57421
_olex2_submission_special_instructions 'No special instructions were received'