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_7701232
_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
'(C156 H114 Cu12 O54 P6), 10(O), O, (Cl -), (C2 H8 N +)'
_chemical_formula_sum            'C158 H122 Cl Cu12 N O65 P6'
_chemical_formula_weight         4058.31
_chemical_name_common            UHM-62
_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
_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                   18.3318(4)
_cell_length_b                   25.8343(5)
_cell_length_c                   33.4448(6)
_cell_measurement_reflns_used    20450
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.2010
_cell_measurement_theta_min      3.9440
_cell_volume                     15839.1(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_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4127
_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    -58.00 -10.00   1.00   30.00    --  -42.10 -77.00  30.00   48
  2  \w   -115.00 -88.00   1.00   30.00    --  -42.10 -38.00 -30.00   27
  3  \w    -87.00 -18.00   1.00   30.00    --  -42.10 -38.00 -30.00   69
  4  \w   -118.00 -10.00   1.00   30.00    --  -42.10 -77.00-150.00  108
  5  \w   -115.00 -10.00   1.00   30.00    --  -42.10 -77.00 -60.00  105
  6  \w    -67.00 -10.00   1.00   30.00    --  -42.10 -77.00 120.00   57
  7  \w   -100.00  -4.00   1.00   30.00    --  -42.10 -19.00  30.00   96
  8  \w    -70.00  29.00   1.00   30.00    --  -42.10  57.00 -30.00   99
  9  \w    -39.00  29.00   1.00   30.00    --  -42.10  38.00  90.00   68
 10  \w    -30.00  70.00   1.00   30.00    --   42.10 -57.00 150.00  100
 11  \w     30.00  97.00   1.00   30.00    --   42.10-125.00  90.00   67
 12  \w     79.00 176.00   1.00  120.00    --  112.00  77.00-150.00   97
 13  \w     79.00 115.00   1.00  120.00    --  112.00  77.00 120.00   36
 14  \w    116.00 172.00   1.00  120.00    --  112.00  77.00 120.00   56
 15  \w     79.00 155.00   1.00  120.00    --  112.00  77.00 -30.00   76
 16  \w     83.00 108.00   1.00  120.00    --  112.00 -94.00 150.00   25
 17  \w     36.00 116.00   1.00  120.00    --  112.00-111.00-120.00   80
 18  \w     82.00 177.00   1.00  120.00    --  112.00  67.00 154.57   95
 19  \w     79.00 105.00   1.00  120.00    --  112.00  77.00  30.00   26
 20  \w     83.00 177.00   1.00  120.00    --  112.00  61.00  90.00   94
 21  \w     83.00 110.00   1.00  120.00    --  112.00  61.00 -30.00   27
 22  \w     29.00  67.00   1.00  120.00    --  112.00 -94.00 150.00   38
 23  \w    112.00 177.00   1.00  120.00    --  112.00  77.00-120.00   65
 24  \w     79.00 149.00   1.00  120.00    --  112.00  77.00 -90.00   70
 25  \w     83.00 109.00   1.00  120.00    --  112.00  61.00 120.00   26
 26  \w     45.00 145.00   1.00  120.00    --  112.00 -77.00-120.00  100
 27  \w     83.00 109.00   1.00  120.00    --  112.00  61.00 -60.00   26
 28  \w     83.00 109.00   1.00  120.00    --  112.00  61.00  30.00   26
 29  \w     83.00 109.00   1.00  120.00    --  112.00  61.00   0.00   26
 30  \w     83.00 140.00   1.00  120.00    --  112.00  61.00  60.00   57
 31  \w     79.00 105.00   1.00  120.00    --  112.00  77.00-180.00   26
 32  \w     79.00  86.00   1.00  120.00    --  112.00 -94.00 -30.00    7
;
_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      0.0387168000
_diffrn_orient_matrix_UB_12      0.0097672000
_diffrn_orient_matrix_UB_13      -0.0514009000
_diffrn_orient_matrix_UB_21      -0.0650969000
_diffrn_orient_matrix_UB_22      0.0262554000
_diffrn_orient_matrix_UB_23      -0.0163409000
_diffrn_orient_matrix_UB_31      0.0363942000
_diffrn_orient_matrix_UB_32      0.0365650000
_diffrn_orient_matrix_UB_33      0.0254317000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            82547
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.492
_diffrn_reflns_theta_max         67.492
_diffrn_reflns_theta_min         3.421
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.634
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90019
_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    0.851
_exptl_crystal_description       block
_exptl_crystal_F_000             4104
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.821
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         7657
_refine_ls_number_restraints     494
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0625
_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^)+(0.1343P)^2^+10.7141P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1937
_refine_ls_wR_factor_ref         0.2037
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6198
_reflns_number_total             7657
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03044a2.cif
_cod_data_source_block           UHM-62
_cod_depositor_comments
'Adding full bibliography for 7701221--7701232.cif.'
_cod_database_code               7701232
_shelx_shelxl_version_number     2018/3
_cell_oxdiff_length_a            18.3350(4)
_cell_oxdiff_length_b            25.8325(6)
_cell_oxdiff_length_c            33.4452(6)
_cell_oxdiff_angle_alpha         90.0234(17)
_cell_oxdiff_angle_beta          89.9865(18)
_cell_oxdiff_angle_gamma         90.0076(19)
_cell_oxdiff_volume              15841.0(6)
_cell_oxdiff_measurement_reflns_used 20453
_shelx_estimated_absorpt_t_min   0.828
_shelx_estimated_absorpt_t_max   0.908
_oxdiff_exptl_absorpt_empirical_full_min 0.682
_oxdiff_exptl_absorpt_empirical_full_max 1.730
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              39090
_shelx_fab_checksum              88974