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_7701231
_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
'(C204 H114 Cu12 O54 P6), 10(O), 2(O), 0.53(O), 0.47(Cl -), 0.47(C2 H8 N +)'
_chemical_formula_sum            'C204.94 H117.76 Cl0.47 Cu12 N0.47 O66.53 P6'
_chemical_formula_weight         4615.80
_chemical_name_common            UHM-63
_space_group_crystal_system      orthorhombic
_space_group_IT_number           71
_space_group_name_Hall           '-I 2 2'
_space_group_name_H-M_alt        'I m m m'
_symmetry_space_group_name_Hall  '-I 2 2'
_symmetry_space_group_name_H-M   'I m m m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_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                90
_cell_formula_units_Z            2
_cell_length_a                   18.6420(4)
_cell_length_b                   25.2812(4)
_cell_length_c                   33.3107(6)
_cell_measurement_reflns_used    9786
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.0350
_cell_measurement_theta_min      3.9330
_cell_volume                     15699.1(5)
_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 10.4127
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_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   -104.00 -79.00   1.00   35.00    --  -42.35 -57.00 -60.00   25
  2  \w    -63.00 -10.00   1.00   35.00    --  -42.35 -77.00 -90.00   53
  3  \w   -117.00 -19.00   1.00   35.00    --  -42.35 -38.00  90.00   98
  4  \w    -67.00 -11.00   1.00   35.00    --  -42.35 -77.00 150.00   56
  5  \w    -51.00 -10.00   1.00   35.00    --  -42.35 -77.00  60.00   41
  6  \w    -57.00 -13.00   1.00   35.00    --  -42.35 -77.00-150.00   44
  7  \w    -58.00 -14.00   1.00   35.00    --  -42.35 -57.00 -60.00   44
  8  \w    -95.00  -2.00   1.00   35.00    --  -42.35 125.00-180.00   93
  9  \w   -104.00 -70.00   1.00   35.00    --  -42.35 -77.00  60.00   34
 10  \w   -118.00 -84.00   1.00   35.00    --  -42.35 -77.00   0.00   34
 11  \w   -119.00 -71.00   1.00   35.00    --  -42.35 -77.00 -90.00   48
 12  \w    -43.00 -10.00   1.00   35.00    --  -42.35 -77.00   0.00   33
 13  \w      3.00  56.00   1.00   35.00    --   42.35 -99.00 120.00   53
 14  \w     24.00  85.00   1.00   35.00    --   42.35-125.00   0.00   61
 15  \w      3.00 112.00   1.00   35.00    --   42.35  19.00-120.00  109
 16  \w     18.00 109.00   1.00  140.00    --  100.87 -94.00  30.00   91
 17  \w     72.00 156.00   1.00  140.00    --  100.87  61.00 -90.00   84
 18  \w     71.00 125.00   1.00  140.00    --  100.87  65.00-142.43   54
 19  \w     72.00 172.00   1.00  140.00    --  100.87  61.00-180.00  100
 20  \w     74.00 149.00   1.00  140.00    --  100.87  61.00 150.00   75
 21  \w    120.00 169.00   1.00  140.00    --  100.87  73.00  42.89   49
 22  \w     69.00  95.00   1.00  140.00    --  100.87  73.00 -88.24   26
 23  \w     28.00  73.00   1.00  140.00    --  100.87 -45.00  30.00   45
;
_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      -0.0545309000
_diffrn_orient_matrix_UB_12      0.0219702000
_diffrn_orient_matrix_UB_13      -0.0304823000
_diffrn_orient_matrix_UB_21      0.0599778000
_diffrn_orient_matrix_UB_22      0.0048443000
_diffrn_orient_matrix_UB_23      -0.0316197000
_diffrn_orient_matrix_UB_31      -0.0159969000
_diffrn_orient_matrix_UB_32      -0.0566301000
_diffrn_orient_matrix_UB_33      -0.0145190000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0770
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_Laue_measured_fraction_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            58750
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.491
_diffrn_reflns_theta_max         67.491
_diffrn_reflns_theta_min         3.497
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.664
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81102
_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            blue
_exptl_crystal_density_diffrn    0.976
_exptl_crystal_description       block
_exptl_crystal_F_000             4658
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.040
_refine_diff_density_min         -1.206
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.209
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         7346
_refine_ls_number_restraints     426
_refine_ls_restrained_S_all      1.209
_refine_ls_R_factor_all          0.1552
_refine_ls_R_factor_gt           0.1168
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3273
_refine_ls_wR_factor_ref         0.3726
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3745
_reflns_number_total             7346
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03044a2.cif
_cod_data_source_block           UHM-63
_cod_depositor_comments
'Adding full bibliography for 7701221--7701232.cif.'
_cod_database_code               7701231
_shelx_shelxl_version_number     2018/3
_cell_oxdiff_length_a            18.6453(5)
_cell_oxdiff_length_b            25.2819(4)
_cell_oxdiff_length_c            33.3039(8)
_cell_oxdiff_angle_alpha         89.9864(16)
_cell_oxdiff_angle_beta          89.970(2)
_cell_oxdiff_angle_gamma         89.9818(18)
_cell_oxdiff_volume              15699.0(6)
_cell_oxdiff_measurement_reflns_used 9786
_shelx_estimated_absorpt_t_min   0.732
_shelx_estimated_absorpt_t_max   0.878
_oxdiff_exptl_absorpt_empirical_full_min 0.705
_oxdiff_exptl_absorpt_empirical_full_max 1.412
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              72314
_shelx_fab_checksum              70300