Vibrational mode analysis of hydrogen-bonded organic frameworks (HOFs): synchrotron infrared studies
Ennis, Courtney; Appadoo, Dominique R. T.; Boer, Stephanie A.; White, Nicholas G.; Physical Chemistry Chemical Physics  (2022) –; doi:10.1039/D2CP00796G

data_7244870
_publ_section_title
;
 Vibrational mode analysis of hydrogen-bonded organic frameworks (HOFs):
 synchrotron infrared studies
;
_journal_name_full               'Physical Chemistry Chemical Physics'
_journal_paper_doi               10.1039/D2CP00796G
_journal_year                    2022
_chemical_compound_source        synthesized
_chemical_formula_moiety         'C28 H32 N8 Si, C28 H16 O8 Si, 12(H2 O)'
_chemical_formula_sum            'C56 H72 N8 O20 Si2'
_chemical_formula_weight         1233.40
_space_group_IT_number           86
_space_group_name_Hall           '-P 4bc'
_space_group_name_H-M_alt        'P 42/n :2'
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_update_record
;
2022-02-13 deposited with the CCDC.	2022-04-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   14.33058(3)
_cell_length_b                   14.33058(3)
_cell_length_c                   8.35856(2)
_cell_measurement_reflns_used    3802
_cell_measurement_temperature    150
_cell_measurement_theta_max      73.5
_cell_measurement_theta_min      6.00
_cell_volume                     1716.560(7)
_computing_cell_refinement       'CrysAlisPro, (Agilent, 2011)'
_computing_data_collection       'CrysAlisPro, (Agilent, 2011'
_computing_data_reduction        'CrysAlisPro, (Agilent, 2011)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction Supernova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.093
_diffrn_reflns_av_unetI/netI     0.013
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            14784
_diffrn_reflns_theta_full        71.766
_diffrn_reflns_theta_max         73.539
_diffrn_reflns_theta_min         4.363
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.077
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.60
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro, (Agilent, 2011)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       shard
_exptl_crystal_F_000             652
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Water/ethanol'
_exptl_crystal_size_max          0.68
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.58
_refine_diff_density_min         -0.44
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0673
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     132
_refine_ls_number_reflns         1393
_refine_ls_number_restraints     92
_refine_ls_R_factor_all          0.0955
_refine_ls_R_factor_gt           0.0938
_refine_ls_shift/su_max          0.0000897
_refine_ls_shift/su_mean         0.0000147
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.06P)^2^ + 8.16P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2334
_refine_ls_wR_factor_gt          0.2318
_refine_ls_wR_factor_ref         0.1977
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              10
_reflns_limit_l_min              0
_reflns_number_gt                1582
_reflns_number_total             1688
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.07
_oxford_diffrn_Wilson_scale      0.02
_oxford_refine_ls_r_factor_ref   0.0845
_oxford_refine_ls_scale          7.0(5)
_oxford_reflns_number_all        1636
_cod_data_source_file            d2cp00796g2.cif
_cod_data_source_block           3
_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 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        1716.560(8)
_cod_original_sg_symbol_H-M      'P 42/n '
_cod_database_code               7244870
_oxford_refine_reflns_threshold_expression_ref I>-3.0\s(I)