A new set of metal-organic frameworks synthesised from diisophthalate-based, 2'-phosphorus-substituted m-terphenyl linker molecules.
Stein, Timo; Hoffmann, Frank; Fröba, Michael; Dalton transactions (Cambridge, England : 2003) 48 (2019) 15127–15135; doi:10.1039/c9dt03044a

data_7701228
_publ_section_title
;
 A new set of metal-organic frameworks synthesised from
 diisophthalate-based, 2'-phosphorus-substituted m-terphenyl linker
 molecules.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15127
_journal_page_last               15135
_journal_paper_doi               10.1039/c9dt03044a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         '(C34 H23 Mg2 O13.57 P), (C3 H7 N O)'
_chemical_formula_sum            'C37 H30 Mg2 N O14.57 P'
_chemical_formula_weight         801.35
_chemical_name_common            UHM-80
_space_group_crystal_system      trigonal
_space_group_IT_number           160
_space_group_name_Hall           'R 3 -2"'
_space_group_name_H-M_alt        'R 3 m :H'
_symmetry_space_group_name_Hall  'R 3 -2"'
_symmetry_space_group_name_H-M   'R 3 m :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-07-24 deposited with the CCDC.    2019-08-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   25.5448(4)
_cell_length_b                   25.5448(4)
_cell_length_c                   21.0016(4)
_cell_measurement_reflns_used    12226
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      51.5240
_cell_measurement_theta_min      4.5160
_cell_volume                     11868.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2063
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -73.00  28.00   1.00   25.00    --    0.00 -57.00   0.00  101
  2  \w    -28.00  73.00   1.00   25.00    --    0.00  57.00   0.00  101
  3  \w    -76.00  33.00   1.00   25.00    --    0.00 -77.00 -90.00  109
  4  \w     29.00 138.00   1.00   50.00    --   61.65  77.00-140.61  109
  5  \w      1.00 103.00   1.00   50.00    --   61.65 -99.00 -90.00  102
  6  \w     29.00 137.00   1.00   50.00    --   61.65  76.00  92.30  108
  7  \w    -11.00  90.00   1.00   50.00    --   61.65 -57.00 -60.00  101
  8  \w     29.00 138.00   1.00   50.00    --   61.65  77.00 -60.00  109
  9  \w     29.00 138.00   1.00   50.00    --   61.65  77.00  30.00  109
 10  \w     23.00 118.00   1.00   50.00    --   61.65-125.00 150.00   95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0565251000
_diffrn_orient_matrix_UB_12      0.0146741000
_diffrn_orient_matrix_UB_13      0.0395791000
_diffrn_orient_matrix_UB_21      -0.0376417000
_diffrn_orient_matrix_UB_22      -0.0150568000
_diffrn_orient_matrix_UB_23      0.0616088000
_diffrn_orient_matrix_UB_31      -0.0154532000
_diffrn_orient_matrix_UB_32      -0.0663568000
_diffrn_orient_matrix_UB_33      -0.0051986000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20838
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        51.528
_diffrn_reflns_theta_max         51.528
_diffrn_reflns_theta_min         4.518
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.141
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.009
_exptl_crystal_description       plate
_exptl_crystal_F_000             3731
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.598
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details
;
 Flack x determined using 1256 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.043(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         3130
_refine_ls_number_restraints     254
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0785
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1380P)^2^+30.0613P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1908
_refine_ls_wR_factor_ref         0.1975
_reflns_Friedel_coverage         0.985
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                2853
_reflns_number_total             3130
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03044a2.cif
_cod_data_source_block           UHM-80
_cod_depositor_comments
'Adding full bibliography for 7701221--7701232.cif.'
_cod_original_cell_volume        11868.3(4)
_cod_database_code               7701228
_shelx_shelxl_version_number     2018/3
_cell_oxdiff_length_a            25.5326(10)
_cell_oxdiff_length_b            25.5477(9)
_cell_oxdiff_length_c            20.9854(8)
_cell_oxdiff_angle_alpha         89.985(3)
_cell_oxdiff_angle_beta          89.993(3)
_cell_oxdiff_angle_gamma         119.968(4)
_cell_oxdiff_volume              11858.6(8)
_cell_oxdiff_measurement_reflns_used 12225
_shelx_estimated_absorpt_t_min   0.847
_shelx_estimated_absorpt_t_max   0.967
_oxdiff_exptl_absorpt_empirical_full_min 0.621
_oxdiff_exptl_absorpt_empirical_full_max 1.417
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              69831
_shelx_fab_checksum              15966