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_7241357
_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_formula_moiety         'C18 H30 Cs N10 Nd O7 Re6 S8'
_chemical_formula_sum            'C18 H30 Cs N10 Nd O7 Re6 S8'
_chemical_formula_weight         2152.23
_space_group_crystal_system      orthorhombic
_space_group_IT_number           66
_space_group_name_Hall           '-C 2 2c'
_space_group_name_H-M_alt        'C c c m'
_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                90
_cell_formula_units_Z            4
_cell_length_a                   10.7133(7)
_cell_length_b                   18.9023(11)
_cell_length_c                   21.6443(13)
_cell_measurement_reflns_used    9948
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      30.87
_cell_measurement_theta_min      2.38
_cell_volume                     4383.1(5)
_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      150.15
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.941
_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  0.0240
_diffrn_reflns_av_unetI/netI     0.0152
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            24302
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        25.250
_diffrn_reflns_theta_max         30.871
_diffrn_reflns_theta_min         2.155
_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    18.908
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6054
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0613 before and 0.0373 after correction.
The Ratio of minimum to maximum transmission is 0.8114.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    3.261
_exptl_crystal_description       block
_exptl_crystal_F_000             3834
_exptl_crystal_size_max          0.205
_exptl_crystal_size_mid          0.149
_exptl_crystal_size_min          0.122
_refine_diff_density_max         1.175
_refine_diff_density_min         -1.888
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.175
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         3343
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.175
_refine_ls_R_factor_all          0.0186
_refine_ls_R_factor_gt           0.0172
_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^)+(0.0068P)^2^+50.6371P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0374
_refine_ls_wR_factor_ref         0.0377
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3218
_reflns_number_total             3343
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01240h2.cif
_cod_data_source_block           lit96nd
_cod_database_code               7241357
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. 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
2. Others
 Fixed Sof: Cs1(0.25) O1M(0.75) H1MA(0.75) H1MB(0.75) O1(0.04)
3.a Rotating group:
 O1M(H1MA,H1MB)
3.b Secondary CH2 refined with riding coordinates:
 C2A(H2AA,H2AB), C3A(H3AA,H3AB)
3.c X=CH2 refined with riding coordinates:
 N1A(H1AA,H1AB)
;
_shelx_res_checksum              31831
_olex2_submission_special_instructions 'No special instructions were received'