Crystal structure of tetraaqua-bis(ethanol-κO)-tetrakis(μ2-trifluoroacetate-κ2O:O′)-bis(trifluoroacetate-κ2O)digadolinium(III) Gd2C16H20O18F18
Ling, Bo-Kai; Huang, Ling-Yu; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 879–880; doi:10.1515/ncrs-2023-0253

data_8107589
_publ_section_title
;
 Crystal structure of
 tetraaqua-bis(ethanol-\kO)-tetrakis(\m2-trifluoroacetate-\k2O:O&#x2032;)-bis(trifluoroacetate-\k2O)digadolinium(III)
 Gd2C16H20O18F18
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              879
_journal_page_last               880
_journal_paper_doi               10.1515/ncrs-2023-0253
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'C16 H20 F18 Gd2 O18'
_chemical_formula_sum            'C16 H20 F18 Gd2 O18'
_chemical_formula_weight         1156.82
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                78.156(5)
_cell_angle_beta                 72.483(5)
_cell_angle_gamma                62.797(4)
_cell_formula_units_Z            1
_cell_length_a                   8.652(3)
_cell_length_b                   9.204(4)
_cell_length_c                   12.305(5)
_cell_measurement_reflns_used    6649
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      28.76
_cell_measurement_theta_min      2.50
_cell_volume                     828.4(6)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.890
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.890
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9812
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.890
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.916
_diffrn_reflns_theta_min         1.741
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.141
_exptl_absorpt_correction_T_max  0.661
_exptl_absorpt_correction_T_min  0.454
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0710 before and 0.0302 after correction.
The Ratio of minimum to maximum transmission is 0.7826.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.319
_exptl_crystal_density_meas      .
_exptl_crystal_description       block
_exptl_crystal_F_000             550
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.069
_refine_diff_density_min         -0.823
_refine_diff_density_rms         0.117
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         3894
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0227
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0274P)^2^+1.0587P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0539
_refine_ls_wR_factor_ref         0.0554
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3639
_reflns_number_total             3894
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0253_suppl_001.cif
_cod_data_source_block           gd-dimer-3f
_cod_database_code               8107589
_shelx_estimated_absorpt_t_max   0.682
_shelx_estimated_absorpt_t_min   0.491
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O7-H7
 0.85 with sigma of 0.01
 C3-H7
 1.898808 with sigma of 0.02
 Gd1-H7
 2.838772 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F5 \\sim C5: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
4. Others
 Fixed Sof: F3(0.65) F7(0.65) F2(0.65) F9(0.35) F5(0.35) F11(0.35)
5.a Rotating group:
 O8(H8A,H8B), O9(H9A,H9B)
5.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B)
5.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
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_shelx_res_checksum              65103
_shelx_hkl_checksum              24443
_olex2_submission_special_instructions 'No special instructions were received'
_publcif_info_exptl_table_max_cols 4
_publcif_info_exptl_table_use_headnotes n
_publcif_funding_html
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