The elusive crystals of calcium acetate hemihydrate: chiral rods linked by parallel hydrophilic strips
Abrahams, Brendan F.; Commons, Christopher J.; Hudson, Timothy A.; Sanchez Arlt, Robin W.; CrystEngComm 23 (2021) 707–713; doi:10.1039/D0CE01590C

data_7241751
_publ_section_title
;
 The elusive crystals of calcium acetate hemihydrate: chiral rods linked
 by parallel hydrophilic strips
;
_journal_issue                   3
_journal_name_full               CrystEngComm
_journal_page_first              707
_journal_page_last               713
_journal_paper_doi               10.1039/D0CE01590C
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C8 H14 Ca2 O9'
_chemical_formula_sum            'C8 H14 Ca2 O9'
_chemical_formula_weight         334.35
_space_group_crystal_system      tetragonal
_space_group_IT_number           142
_space_group_name_Hall           '-I 4bd 2c'
_space_group_name_H-M_alt        'I 41/a c d :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-29
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6186)
;
_audit_update_record
;
2020-11-29 deposited with the CCDC.	2020-12-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            32
_cell_length_a                   33.1757(4)
_cell_length_b                   33.1757(4)
_cell_length_c                   10.5521(2)
_cell_measurement_reflns_used    4250
_cell_measurement_temperature    130.01(10)
_cell_measurement_theta_max      75.1560
_cell_measurement_theta_min      5.1200
_cell_volume                     11613.9(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      130.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2273
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -9.00  32.00   1.00   15.00    --  -41.87  38.00-120.00   41
  2  \w    -52.00  38.00   1.00   15.00    --  -41.87  19.00-150.00   90
  3  \w     31.00  88.00   1.00   30.00    --  109.15 -94.00 150.00   57
  4  \w     42.00  69.00   1.00   30.00    --  109.15 -30.00  30.00   27
  5  \w     34.00  76.00   1.00   30.00    --  109.15 -30.00 -60.00   42
  6  \w     47.00  97.00   1.00   30.00    --  109.15 -45.00-120.00   50
  7  \w    102.00 172.00   1.00   30.00    --  109.15  95.00 -10.00   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0396660000
_diffrn_orient_matrix_UB_12      -0.0164571000
_diffrn_orient_matrix_UB_13      0.0566101000
_diffrn_orient_matrix_UB_21      -0.0222603000
_diffrn_orient_matrix_UB_22      0.0106439000
_diffrn_orient_matrix_UB_23      -0.1234775000
_diffrn_orient_matrix_UB_31      0.0097509000
_diffrn_orient_matrix_UB_32      -0.0419899000
_diffrn_orient_matrix_UB_33      -0.0536423000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            12099
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.034
_diffrn_reflns_theta_min         3.769
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.182
_exptl_absorpt_correction_T_max  0.900
_exptl_absorpt_correction_T_min  0.475
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_description       block
_exptl_crystal_F_000             5568
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.137
_exptl_crystal_size_min          0.061
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.000027(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.180
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         2761
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.183
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0293
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0472P)^2^+5.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0794
_refine_ls_wR_factor_ref         0.0829
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2498
_reflns_number_total             2761
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01590c2.cif
_cod_data_source_block           gaussian_abs
_cod_depositor_comments          'Adding full bibliography for 7241751.cif.'
_cod_original_cell_volume        11613.9(4)
_cod_original_sg_symbol_H-M      'I 41/a c d'
_cod_database_code               7241751
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ca2 C8 H14 O9'
_shelx_estimated_absorpt_t_max   0.668
_shelx_estimated_absorpt_t_min   0.412
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All O(H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O9-H9C = O9-H9B = O9-H9A
 0.83 with sigma of 0.02
 H9A-H9C = H9B-H9A = H9B-H9C
 1.34 with sigma of 0.04
3. Others
 Sof(O7B)=1-FVAR(1)
 Sof(O7A)=FVAR(1)
 Fixed Sof: H9A(0.75) H9B(0.75) H9C(0.5)
4.a Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              51183
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.436
_oxdiff_exptl_absorpt_empirical_full_min 0.682