Metal-organic frameworks with solvent-free lanthanide coordination environments: synthesis from aqueous ethanol solutions
Litvinova, Yulia M.; Gayfulin, Yakov M.; Brylev, Konstantin; Piryazev, Dmitry A.; van Leusen, Jan; Kögerler, Paul; Mironov, Yuri V.; CrystEngComm  (2020) –; doi:10.1039/D0CE01240H

data_7241358
_publ_section_title
;
 Metal-organic frameworks with solvent-free lanthanide coordination
 environments: synthesis from aqueous ethanol solutions
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE01240H
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C18 H30 Cs N10 O7 Re6 Se8 Tb'
_chemical_formula_sum            'C18 H30 Cs N10 O7 Re6 Se8 Tb'
_chemical_formula_weight         2521.21
_space_group_crystal_system      hexagonal
_space_group_IT_number           181
_space_group_name_Hall           'P 64 2 (0 0 2)'
_space_group_name_H-M_alt        'P 64 2 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-01-23
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2020-06-23 deposited with the CCDC.	2020-10-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   10.8248(17)
_cell_length_b                   10.8248(17)
_cell_length_c                   32.123(5)
_cell_measurement_reflns_used    9842
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      29.81
_cell_measurement_theta_min      2.17
_cell_volume                     3259.8(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX2 CCD area detector'
_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  0.0785
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            20952
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.172
_diffrn_source                   'sealed tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    25.813
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.3405
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1466 before and 0.0796 after correction.
The Ratio of minimum to maximum transmission is 0.4564.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.853
_exptl_crystal_description       plate
_exptl_crystal_F_000             3288
_exptl_crystal_size_max          0.235
_exptl_crystal_size_mid          0.204
_exptl_crystal_size_min          0.061
_refine_diff_density_max         4.567
_refine_diff_density_min         -3.466
_refine_diff_density_rms         0.418
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.09(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     123
_refine_ls_number_reflns         2508
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0448
_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^)+(0.0324P)^2^+175.8010P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1108
_reflns_Friedel_coverage         0.589
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2247
_reflns_number_total             2508
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01240h2.cif
_cod_data_source_block           qqq_a
_cod_original_cell_volume        3259.7(11)
_cod_original_sg_symbol_Hall     'P 64 2c (0 0 -1)'
_cod_database_code               7241358
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.302
_shelx_estimated_absorpt_t_min   0.065
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.91(6)
 0.09(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Uiso/Uaniso restraints and constraints
N1 \\sim C1: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01
within 2A
N2 \\sim C2: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01
within 2A
Uanis(O1M) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C2) \\sim Ueq, Uanis(N2) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N2) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Others
 Fixed Sof: Cs1(0.25) O1M(0.5) H1MA(0.5) H1MB(0.5) C3AB(0.65) H3AA(0.65)
 H3AB(0.65) C2AB(0.65) H2AA(0.65) H2AB(0.65) C2AA(0.35) H2AC(0.35) H2AD(0.35)
 C3AA(0.35) H3AC(0.35) H3AD(0.35)
5.a Rotating group:
 O1M(H1MA,H1MB)
5.b Secondary CH2 refined with riding coordinates:
 C3AB(H3AA,H3AB), C2AB(H2AA,H2AB), C2AA(H2AC,H2AD), C3AA(H3AC,H3AD)
5.c X=CH2 refined with riding coordinates:
 N1A(H1AA,H1AB)
;
_shelx_res_checksum              37019
_olex2_submission_special_instructions 'No special instructions were received'