Analysis of charge density in nonaaquagadolinium(III) trifluoromethanesulfonate – insight into Gd^III^—OH~2~ bonding
Janicki, Rafał; Starynowicz, Przemysław; Acta Crystallographica Section B 76 (2020) –; doi:10.1107/S2052520620006903

data_2108622
_publ_section_title
;
 Analysis of charge density in nonaaquagadolinium(III)
 trifluoromethanesulfonate -- insight into Gd^III^---OH~2~ bonding
;
_journal_coeditor_code           PX5020SUP1
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520620006903
_journal_volume                  76
_journal_year                    2020
_chemical_formula_sum            'C3 H18 F9 Gd O18 S3'
_chemical_formula_weight         766.60
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   'P 63/m'
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             '22-Apr-20 T13:07:21-00:00'
_audit_creation_method           'XD routine XDCIF'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   13.7828(9)
_cell_length_b                   13.7828(9)
_cell_length_c                   7.3148(5)
_cell_measurement_reflns_used    61419
_cell_measurement_temperature    80(1)
_cell_measurement_theta_max      69.7670
_cell_measurement_theta_min      2.7850
_cell_volume                     1203.39(14)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Volkov et al, (2006)'
_computing_publication_material  'Volkov et al, (2006)'
_computing_structure_refinement  'Volkov et al, (2006)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      80(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3456
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_max 0.9981
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_av_sigmaI/netI    0.0254
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            86103
_diffrn_reflns_reduction_process
;
 Scaled and merged with SORTAV
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_max         69.798
_diffrn_reflns_theta_min         1.706
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.143
_exptl_absorpt_correction_T_max  0.542
_exptl_absorpt_correction_T_min  0.401
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_description       irregular
_exptl_crystal_F_000             746
_exptl_crystal_size_max          0.424
_exptl_crystal_size_mid          0.355
_exptl_crystal_size_min          0.286
_refine_diff_density_max         0.678
_refine_diff_density_min         -0.726
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       0.441(4)
_refine_ls_extinction_expression
;
        Becker, P.J. & Coppens, P. (1974) Acta Cryst., A30, 129-153.
;
_refine_ls_extinction_method     'Becker-Coppens type 1 Lorentzian isotropic'
_refine_ls_goodness_of_fit_ref   1.837
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         5325
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.012
_refine_ls_R_factor_gt           0.009
_refine_ls_shift/su_max          0.00035
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;    calc w2 = q/[s^2^(Fo^2^) + (0.00 P)^2^ + 0.20 P + 0.00 + 0.00 sin(th)]
     where P = (0.3333 Fo^2^ + 0.6667 Fc^2^)
           q = 1.0
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.023
_reflns_number_gt                7966
_reflns_number_total             8039
_cod_data_source_file            px5020sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      P6(3)/m
_cod_database_code               2108622
_oxdiff_exptl_absorpt_empirical_full_min 0.940
_oxdiff_exptl_absorpt_empirical_full_max 1.095