Crystal Structures of CuCl2·2H2O (Eriochalcite) and NiCl2∙6H2O (Nickelbischofite) at Low Temperature: Full Refinement of Hydrogen Atoms Using Non-Spherical Atomic Scattering Factors
Boeré, René T.; Crystals 13 (2023) 293–; doi:10.3390/cryst13020293

data_1568587
_publ_section_title
;
 Crystal Structures of CuCl2&#x00B7;2H2O (Eriochalcite) and
 NiCl2&#x2219;6H2O (Nickelbischofite) at Low Temperature: Full Refinement
 of Hydrogen Atoms Using Non-Spherical Atomic Scattering Factors
;
_journal_issue                   2
_journal_name_full               Crystals
_journal_page_first              293
_journal_paper_doi               10.3390/cryst13020293
_journal_volume                  13
_journal_year                    2023
_chemical_formula_moiety         'Cl2 Cu H4 O2'
_chemical_formula_sum            'Cl2 Cu H4 O2'
_chemical_formula_weight         170.481
_space_group_crystal_system      orthorhombic
_space_group_IT_number           53
_space_group_name_Hall           '-P 2ac 2'
_space_group_name_H-M_alt        'P m n a'
_symmetry_Int_Tables_number      53
_atom_sites_solution_primary     dual
_audit_creation_date             2023-01-25
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2022.11.02 svn.ra8b101fa for OlexSys, GUI svn.r6635)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.0553(3)
_cell_length_b                   3.7295(2)
_cell_length_c                   7.3674(3)
_cell_measurement_reflns_used    9941
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      37.8640
_cell_measurement_theta_min      2.7030
_cell_volume                     221.333(17)
_computing_cell_refinement       'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-alpha (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 1.0000
_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    -44.00  26.00   0.50    1.39    --   22.41 -38.00 150.00  140
  2  \w     11.00  85.00   0.50    1.39    --   22.41  57.00  60.00  148
  3  \w     39.00  91.00   0.50    1.39    --   22.41 178.00 -90.00  104
  4  \w    -15.00  58.00   0.50    1.39    --   22.41 -99.00 -90.00  146
  5  \w    -47.00  92.00   0.50    1.39    --   22.41   0.00 -60.00  278
  6  \w    -15.00  58.00   0.50    1.39    --   22.41 -99.00 -60.00  146
  7  \w     19.00  89.00   0.50    1.39    --   22.41  38.00  60.00  140
  8  \w     37.00  91.00   0.50    1.39    --   22.41-178.00-180.00  108
  9  \w     16.00  92.00   0.50    1.39    --   22.41  19.00   0.00  152
 10  \w    -89.00 -14.00   0.50    1.39    --  -25.54 -57.00-120.00  150
 11  \w    -92.00 -22.00   0.50    1.39    --  -25.54 -38.00  90.00  140
 12  \w    -93.00 -39.00   0.50    1.39    --  -25.54 150.00 -82.04  108
 13  \w    -14.00  12.00   0.50    1.39    --  -25.54-102.00 127.99   52
 14  \w    -14.00  13.00   0.50    1.39    --  -25.54-103.00 171.28   54
 15  \w    -36.00  -6.00   0.50    1.39    --  -25.54 -73.00 -60.32   60
 16  \w    -89.00 -14.00   0.50    1.39    --  -25.54 -57.00  90.00  150
 17  \w    -29.00   5.00   0.50    1.39    --  -25.54 -90.00  51.40   68
 18  \w    -91.00 -38.00   0.50    1.39    --  -25.54 147.00   5.34  106
 19  \w    -14.00  12.00   0.50    1.39    --  -25.54-102.00 -90.17   52
 20  \w    -22.00   7.00   0.50    1.39    --  -25.54 -93.00-146.39   58
 21  \w    -92.00 -22.00   0.50    1.39    --  -25.54 -38.00 150.00  140
 22  \w    -86.00 -35.00   0.50    1.39    --  -25.54 141.00-115.26  102
 23  \w    -89.00 -14.00   0.50    1.39    --  -25.54 -57.00  30.00  150
 24  \w    -68.00 -15.00   0.50    1.39    --  -25.54 110.00 118.47  106
 25  \w    -79.00 -30.00   0.50    1.39    --  -25.54 128.00  61.94   98
 26  \w    -47.00  92.00   0.50    1.39    --   22.41   0.00 -90.00  278
 27  \w    -47.00  92.00   0.50    1.39    --   22.41   0.00-120.00  278
 28  \w    -47.00 -12.00   0.50    1.39    --   22.41   0.00 -30.00   70
 29  \w    -47.00  92.00   0.50    1.39    --   22.41   0.00 -60.00  278
 30  \w    -44.00  26.00   0.50    1.39    --   22.41 -38.00-120.00  140
 31  \w     39.00  91.00   0.50    1.39    --   22.41 178.00 120.00  104
 32  \w     19.00  89.00   0.50    1.39    --   22.41  38.00   0.00  140
 33  \w    -47.00  92.00   0.50    1.39    --   22.41   0.00-180.00  278
 34  \w    -47.00  92.00   0.50    1.39    --   22.41   0.00-150.00  278
 35  \w    -49.00  21.00   0.50    1.39    --  -25.54  77.00 -30.00  140
 36  \w    -91.00 -38.00   0.50    1.39    --  -25.54 147.00 132.97  106
 37  \w    -15.00  11.00   0.50    1.39    --  -25.54-100.00 -64.18   52
 38  \w    -21.00   8.00   0.50    1.39    --  -25.54 -94.00 -20.15   58
 39  \w    -80.00 -30.00   0.50    1.39    --  -25.54 130.00-152.99  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0455157000
_diffrn_orient_matrix_UB_12      0.1267590000
_diffrn_orient_matrix_UB_13      0.0516455000
_diffrn_orient_matrix_UB_21      -0.0444828000
_diffrn_orient_matrix_UB_22      0.1415811000
_diffrn_orient_matrix_UB_23      -0.0420122000
_diffrn_orient_matrix_UB_31      -0.0609191000
_diffrn_orient_matrix_UB_32      -0.0086526000
_diffrn_orient_matrix_UB_33      0.0694428000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0598
_diffrn_reflns_av_unetI/netI     0.0170
_diffrn_reflns_Laue_measured_fraction_full 1.0000
_diffrn_reflns_Laue_measured_fraction_max 1.0000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            20107
_diffrn_reflns_point_group_measured_fraction_full 1.0000
_diffrn_reflns_point_group_measured_fraction_max 1.0000
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         34.47
_diffrn_reflns_theta_min         3.75
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.967
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.277
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.116a (Rigaku Oxford Diffraction, 2021)
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 greenish blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.558
_exptl_crystal_description       needle
_exptl_crystal_F_000             167.383
_exptl_crystal_size_max          0.211
_exptl_crystal_size_mid          0.038
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.5629
_refine_diff_density_min         -0.4174
_refine_diff_density_rms         0.0779
_refine_ls_d_res_high            0.6279
_refine_ls_d_res_low             5.4365
_refine_ls_goodness_of_fit_ref   1.0159
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     25
_refine_ls_number_reflns         499
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.0095
_refine_ls_R_factor_all          0.0134
_refine_ls_R_factor_gt           0.0120
_refine_ls_shift/su_max          0.0010
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0077P)^2^+0.1322P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0257
_refine_ls_wR_factor_ref         0.0264
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              0
_reflns_limit_k_max              5
_reflns_limit_k_min              0
_reflns_limit_l_max              11
_reflns_limit_l_min              0
_reflns_number_gt                476
_reflns_number_total             499
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            Cu-NiCl2Hydrates_Boere-Crystals.cif
_cod_data_source_block           1a-CuCl2dihydrate-Mo
_cod_database_code               1568587
_chemical_oxdiff_formula         CuCl2H4O2
_chemical_oxdiff_usercomment     Mo
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(H1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
;
_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 1.196
_oxdiff_exptl_absorpt_empirical_full_min 0.809