Fluorinated Linkers Enable the Synthesis of Flexible MOFs with 1D Alkaline Earth SBUs and a Temperature-Induced Phase Transition
Ruschewitz, Uwe; Sebastian, Sean; Dicke, Finn P.; Dalton Transactions  (2023) –; doi:10.1039/D3DT00422H

data_7712781
_publ_section_title
;
 Fluorinated Linkers Enable the Synthesis of Flexible MOFs with 1D
 Alkaline Earth SBUs and a Temperature-Induced Phase Transition
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00422H
_journal_year                    2023
_chemical_compound_source
'Synthesized from calciumnitrate with 3F-BTB in DMF/HOAc mixture'
_chemical_formula_moiety
'(Ca 2+)5 , (C27 H12 O6 F3 3-)3, (C3 H7 N O)5, O, (C2 H3 O2 1-)'
_chemical_formula_sum            'C98 H74 Ca5 F9 N5 O26'
_chemical_formula_weight         2109.02
_chemical_name_common            'UoC-9(Ca), RT'
_chemical_properties_physical    air-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           46
_space_group_name_Hall           'I 2 -2a'
_space_group_name_H-M_alt        'I m a 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/2
_audit_update_record
;
2023-02-09 deposited with the CCDC.	2023-04-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.0050(9)
_cell_length_b                   16.5630(4)
_cell_length_c                   28.8501(15)
_cell_measurement_reflns_used    9531
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      71.14
_cell_measurement_theta_min      2.76
_cell_volume                     15293.4(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT-VERSION 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      300(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1181
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            166449
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.477
_diffrn_reflns_theta_min         3.004
_diffrn_source                   sealed-tube
_exptl_absorpt_coefficient_mu    2.056
_exptl_absorpt_correction_T_max  0.3239
_exptl_absorpt_correction_T_min  0.1764
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction 
 Reference: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.916
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             4344
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DMF'
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.396
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details
;
 Flack x determined using 5551 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.029(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     754
_refine_ls_number_reflns         15359
_refine_ls_number_restraints     388
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0669P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1047
_reflns_Friedel_coverage         0.947
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                13538
_reflns_number_total             15359
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00422h2.cif
_cod_data_source_block           sss186gn_rt_0ma_a_sq
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_database_code               7712781
_shelx_shelxl_version_number     2019/2
_shelx_res_checksum              12283
_shelx_hkl_checksum              44539
_shelx_fab_checksum              79293