Superprotonic Phase Change to a Robust Phosphonate Metal‒Organic Framework
Hassanzadeh Fard, Zohreh; Wong, Norman E.; Malliakas, Christos D.; Ramaswamy, Padmini; Taylor, Jared M.; Otsubo, Kazuya; Shimizu, George K. H.; Chemistry of Materials 30 (2018) 314–; doi:10.1021/acs.chemmater.7b04467

data_4002882
_publ_section_title
;
 Superprotonic Phase Change to a Robust Phosphonate Metal--Organic
 Framework
;
_journal_issue                   2
_journal_name_full               'Chemistry of Materials'
_journal_page_first              314
_journal_paper_doi               10.1021/acs.chemmater.7b04467
_journal_volume                  30
_journal_year                    2018
_chemical_formula_moiety         'C23 H15 N1 F2 O9 P3 Zr, 3(Me2NH2)'
_chemical_formula_sum            'C29 H39 F2 N4 O9 P3 Zr'
_chemical_formula_weight         809.77
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                78.6870(10)
_cell_angle_beta                 83.3360(10)
_cell_angle_gamma                88.4970(10)
_cell_formula_units_Z            2
_cell_length_a                   8.28000(10)
_cell_length_b                   13.9085(2)
_cell_length_c                   15.2215(2)
_cell_measurement_reflns_used    9935
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      54
_cell_measurement_theta_min      3.35
_cell_volume                     1707.26(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21718
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        66.633
_diffrn_reflns_theta_max         66.633
_diffrn_reflns_theta_min         2.980
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.568
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6629
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS from Bruker SAINT'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         5879
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0259
_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^)+(0.0390P)^2^+0.7447P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0641
_refine_ls_wR_factor_ref         0.0668
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5236
_reflns_number_total             5879
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm7b04467_si_002.cif
_cod_data_source_block           Zr-PTAP
_cod_depositor_comments
;
The following automatic conversions were performed:

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

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 4002882.cif.
;
_cod_database_code               4002882
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              81798
_shelx_hkl_checksum              5213