Electron-deficient trifluoromethyl-substituted sub-components affect the properties of M4L4 tetrahedral cages
Struch, Niklas; Topić, Filip; Rissanen, Kari; Lützen, Arne; Dalton Trans.  (2017) –; doi:10.1039/C7DT02182H

data_7043395
_publ_section_title
;
 Electron-deficient trifluoromethyl-substituted sub-components affect the
 properties of M4L4 tetrahedral cages
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02182H
_journal_year                    2017
_chemical_formula_moiety
'C160 H96 F36 Fe4 N24 O4, 0.73(C F3 O3 S), 3.67(F6 P), 5(C2 H3 N)'
_chemical_formula_sum
'C170.72 H111 F60.23 Fe4 N29 O6.17 P3.67 S0.73'
_chemical_formula_weight         4172.09
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-03-28 deposited with the CCDC.
2017-06-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.077(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   39.5026(9)
_cell_length_b                   21.4950(6)
_cell_length_c                   30.4701(9)
_cell_measurement_reflns_used    12239
_cell_measurement_temperature    123.0(1)
_cell_measurement_theta_max      73.5020
_cell_measurement_theta_min      4.1010
_cell_volume                     25872.4(12)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_publication_material
'OLEX2 (Dolomanov et al., 2009) & WinGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.926
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            43952
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.926
_diffrn_reflns_theta_full        67.750
_diffrn_reflns_theta_max         74.335
_diffrn_reflns_theta_min         3.727
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.816
_exptl_absorpt_correction_T_max  0.662
_exptl_absorpt_correction_T_min  0.507
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (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            'dark violet'
_exptl_crystal_density_diffrn    1.071
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             8402
_exptl_crystal_size_max          0.415
_exptl_crystal_size_mid          0.244
_exptl_crystal_size_min          0.190
_refine_diff_density_max         2.543
_refine_diff_density_min         -1.494
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.283
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1479
_refine_ls_number_reflns         24429
_refine_ls_number_restraints     2203
_refine_ls_restrained_S_all      1.283
_refine_ls_R_factor_all          0.1138
_refine_ls_R_factor_gt           0.0965
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2914
_refine_ls_wR_factor_ref         0.3161
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18750
_reflns_number_total             24429
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02182h2.cif
_cod_data_source_block           1
_cod_database_code               7043395
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.388
_shelx_estimated_absorpt_t_max   0.617
_shelx_res_checksum              29450
_shelx_fab_checksum              92704