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_7701223
_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_sum            'C38 H31 O9 P'
_chemical_formula_weight         662.60
_chemical_name_systematic
'(3,3??,5,5??-Tetramethoxycarbonyl-1,1?:3?,1??-terphen-2?-yl)diphenylphosphane oxide'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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                 99.4400(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   36.1084(4)
_cell_length_b                   12.08210(10)
_cell_length_c                   15.1558(2)
_cell_measurement_reflns_used    28734
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.4130
_cell_measurement_theta_min      3.8440
_cell_volume                     6522.41(13)
_computing_cell_refinement       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -50.00  15.00   1.00    3.50    --  -42.10  38.00-120.00   65
  2  \w    -50.00 -14.00   1.00    3.50    --  -42.10 -57.00-150.00   36
  3  \w    -50.00 -10.00   1.00    3.50    --  -42.10 -77.00 -90.00   40
  4  \w    -71.00 -10.00   1.00    3.50    --  -42.10 -77.00-180.00   61
  5  \w    -75.00 -14.00   1.00    3.50    --  -42.10 -57.00   0.00   61
  6  \w      1.00  69.00   1.00    3.50    --   42.10 -99.00 120.00   68
  7  \w      3.00  49.00   1.00    3.50    --   42.10 -99.00  60.00   46
  8  \w      1.00  44.00   1.00    3.50    --   42.10 -99.00   0.00   43
  9  \w     37.00  83.00   1.00   14.00    --  112.00-111.00   0.00   46
 10  \w     77.00 114.00   1.00   14.00    --  112.00-111.00  30.00   37
 11  \w    110.00 145.00   1.00   14.00    --  112.00 -77.00   0.00   35
 12  \w     91.00 116.00   1.00   14.00    --  112.00-111.00 120.00   25
 13  \w     37.00  72.00   1.00   14.00    --  112.00-111.00 120.00   35
 14  \w     37.00 114.00   1.00   14.00    --  112.00-111.00  90.00   77
 15  \w     50.00 116.00   1.00   14.00    --  112.00-111.00 -30.00   66
 16  \w     87.00 116.00   1.00   14.00    --  112.00-111.00 -90.00   29
 17  \w     53.00 139.00   1.00   14.00    --  112.00 -61.00-180.00   86
 18  \w     82.00 114.00   1.00   14.00    --  112.00  64.00 -51.62   32
 19  \w    122.00 178.00   1.00   14.00    --  112.00  77.00 -60.00   56
 20  \w    146.00 173.00   1.00   14.00    --  112.00  77.00   0.00   27
 21  \w    141.00 168.00   1.00   14.00    --  112.00  61.00   7.16   27
 22  \w    134.00 160.00   1.00   14.00    --  112.00  62.00  43.04   26
 23  \w    113.00 176.00   1.00   14.00    --  112.00  77.00  30.00   63
 24  \w    121.00 176.00   1.00   14.00    --  112.00  73.00 -72.45   55
 25  \w    131.00 177.00   1.00   14.00    --  112.00  77.00-120.00   46
 26  \w    114.00 166.00   1.00   14.00    --  112.00  73.00-149.49   52
 27  \w    110.00 176.00   1.00   14.00    --  112.00  77.00-180.00   66
 28  \w     80.00 106.00   1.00   14.00    --  112.00  73.00 -72.45   26
 29  \w     79.00 174.00   1.00   14.00    --  112.00  77.00 -30.00   95
 30  \w    115.00 141.00   1.00   14.00    --  112.00  77.00  60.00   26
 31  \w    109.00 178.00   1.00   14.00    --  112.00  77.00 150.00   69
 32  \w    127.00 163.00   1.00   14.00    --  112.00  60.00 164.26   36
 33  \w     80.00 106.00   1.00   14.00    --  112.00  76.00  49.26   26
 34  \w     79.00 126.00   1.00   14.00    --  112.00  77.00  90.00   47
 35  \w     82.00 173.00   1.00   14.00    --  112.00  67.00 123.37   91
 36  \w     83.00 178.00   1.00   14.00    --  112.00  61.00  60.00   95
 37  \w     83.00 175.00   1.00   14.00    --  112.00  61.00  90.00   92
 38  \w     83.00 120.00   1.00   14.00    --  112.00  61.00 120.00   37
 39  \w     79.00 104.00   1.00   14.00    --  112.00  77.00 150.00   25
 40  \w     83.00 109.00   1.00   14.00    --  112.00  60.00 164.26   26
 41  \w     83.00 145.00   1.00   14.00    --  112.00  61.00 150.00   62
 42  \w     79.00 106.00   1.00   14.00    --  112.00  77.00  30.00   27
 43  \w     79.00 105.00   1.00   14.00    --  112.00  77.00   0.00   26
 44  \w     83.00 165.00   1.00   14.00    --  112.00  61.00   0.00   82
 45  \w     80.00 111.00   1.00   14.00    --  112.00  73.00-149.49   31
 46  \w     83.00 109.00   1.00   14.00    --  112.00  61.00-150.00   26
 47  \w     83.00 149.00   1.00   14.00    --  112.00  61.00-120.00   66
 48  \w     83.00 159.00   1.00   14.00    --  112.00  61.00 -90.00   76
 49  \w     80.00 105.00   1.00   14.00    --  112.00  76.00 -43.98   25
 50  \w     83.00 115.00   1.00   14.00    --  112.00  61.00 -30.00   32
 51  \w     83.00 129.00   1.00   14.00    --  112.00  61.00  30.00   46
 52  \w     79.00 106.00   1.00   14.00    --  112.00  77.00 -60.00   27
 53  \w     82.00 108.00   1.00   14.00    --  112.00  64.00 -77.00   26
 54  \w     79.00 105.00   1.00   14.00    --  112.00  77.00-120.00   26
 55  \w     80.00 107.00   1.00   14.00    --  112.00  77.00-150.00   27
 56  \w     83.00 109.00   1.00   14.00    --  112.00  61.00-180.00   26
 57  \w     79.00 105.00   1.00   14.00    --  112.00  77.00-180.00   26
 58  \w     83.00 109.00   1.00   14.00    --  112.00  61.00   7.16   26
 59  \w     83.00 109.00   1.00   14.00    --  112.00  62.00  43.04   26
 60  \w     79.00 105.00   1.00   14.00    --  112.00  77.00  60.00   26
 61  \w     79.00 105.00   1.00   14.00    --  112.00  77.00 120.00   26
 62  \w     81.00 112.00   1.00   14.00    --  112.00  70.00 178.61   31
 63  \w      7.00  33.00   1.00    3.50    --   42.10  86.00  60.00   26
 64  \w     37.00  91.00   1.00   14.00    --  112.00 -77.00   0.00   54
 65  \w     41.00  66.00   1.00   14.00    --  112.00-111.00 -90.00   25
 66  \w     40.00 112.00   1.00   14.00    --  112.00-111.00-150.00   72
 67  \w     33.00  96.00   1.00   14.00    --  112.00 -94.00 150.00   63
 68  \w    -95.00  -2.00   1.00    3.50    --  -42.10 125.00-150.00   93
 69  \w   -114.00 -88.00   1.00    3.50    --  -42.10 -57.00-150.00   26
 70  \w   -118.00 -79.00   1.00    3.50    --  -42.10 -77.00 -90.00   39
 71  \w   -118.00 -10.00   1.00    3.50    --  -42.10 -77.00 -30.00  108
 72  \w   -103.00 -10.00   1.00    3.50    --  -42.10 -77.00  90.00   93
 73  \w   -116.00 -18.00   1.00    3.50    --  -42.10 -38.00 120.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0265707000
_diffrn_orient_matrix_UB_12      -0.1005188000
_diffrn_orient_matrix_UB_13      0.0138784000
_diffrn_orient_matrix_UB_21      0.0181646000
_diffrn_orient_matrix_UB_22      0.0370187000
_diffrn_orient_matrix_UB_23      -0.0803400000
_diffrn_orient_matrix_UB_31      0.0289076000
_diffrn_orient_matrix_UB_32      0.0691201000
_diffrn_orient_matrix_UB_33      0.0630176000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            66459
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.484
_diffrn_reflns_theta_min         3.863
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.233
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75542
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.42b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_description       plate
_exptl_crystal_F_000             2768
_exptl_crystal_recrystallization_method
'recrystallization from ethanol at 0 \%C'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         6465
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0529P)^2^+6.5889P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0937
_refine_ls_wR_factor_ref         0.0980
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5841
_reflns_number_total             6465
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03044a2.cif
_cod_data_source_block           3dmonoclinic
_cod_depositor_comments
'Adding full bibliography for 7701221--7701232.cif.'
_cod_database_code               7701223
_shelx_shelxl_version_number     2018/3
_cell_oxdiff_length_a            36.1015(7)
_cell_oxdiff_length_b            12.0845(2)
_cell_oxdiff_length_c            15.1557(3)
_cell_oxdiff_angle_alpha         89.9404(15)
_cell_oxdiff_angle_beta          99.4413(16)
_cell_oxdiff_angle_gamma         89.9949(15)
_cell_oxdiff_volume              6522.4(2)
_cell_oxdiff_measurement_reflns_used 28834
_shelx_estimated_absorpt_t_min   0.724
_shelx_estimated_absorpt_t_max   0.964
_oxdiff_exptl_absorpt_empirical_full_min 0.178
_oxdiff_exptl_absorpt_empirical_full_max 1.490
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_theta     74.33
_reflns_odcompleteness_iscentric 1
_shelx_res_checksum              14034