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_7701226
_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      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   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                101.701(3)
_cell_angle_beta                 97.017(3)
_cell_angle_gamma                102.970(4)
_cell_formula_units_Z            2
_cell_length_a                   8.2514(4)
_cell_length_b                   11.6965(5)
_cell_length_c                   17.6863(6)
_cell_measurement_reflns_used    15424
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.1710
_cell_measurement_theta_min      3.9750
_cell_volume                     1603.49(12)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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 5.2063
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.976
_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    -96.00  -2.00   1.00    1.00    --  -41.85 125.00   0.00   94
  2  \w   -116.00 -17.00   1.00    1.00    --  -41.85 -38.00-150.00   99
  3  \w   -122.00  -1.00   1.00    1.00    --  -41.85 -19.00 -90.00  121
  4  \w     23.00  98.00   1.00    1.00    --   41.85-125.00 -30.00   75
  5  \w      1.00  83.00   1.00    1.00    --   41.85 -99.00  90.00   82
  6  \w      1.00  83.00   1.00    1.00    --   41.85 -99.00-180.00   82
  7  \w     36.00 116.00   1.00    4.00    --  112.00-111.00 -30.00   80
  8  \w     36.00 116.00   1.00    4.00    --  112.00-111.00 120.00   80
  9  \w     40.00 141.00   1.00    4.00    --  112.00 -61.00 -60.00  101
 10  \w    100.00 178.00   1.00    4.00    --  112.00 111.00 -30.00   78
 11  \w     29.00 109.00   1.00    4.00    --  112.00 -94.00 150.00   80
 12  \w     29.00 109.00   1.00    4.00    --  112.00 -94.00-120.00   80
 13  \w     36.00 116.00   1.00    4.00    --  112.00-111.00  30.00   80
 14  \w     86.00 178.00   1.00    4.00    --  112.00  45.00  90.00   92
 15  \w     84.00 178.00   1.00    4.00    --  112.00  30.00   0.00   94
 16  \w    100.00 178.00   1.00    4.00    --  112.00 111.00 -90.00   78
 17  \w    100.00 178.00   1.00    4.00    --  112.00 111.00  30.00   78
 18  \w     29.00 109.00   1.00    4.00    --  112.00 -94.00  60.00   80
 19  \w     39.00 138.00   1.00    4.00    --  112.00 -45.00 120.00   99
 20  \w     29.00 109.00   1.00    4.00    --  112.00 -94.00 120.00   80
 21  \w    100.00 178.00   1.00    4.00    --  112.00 111.00 -60.00   78
 22  \w     36.00 116.00   1.00    4.00    --  112.00-111.00-150.00   80
 23  \w     80.00 178.00   1.00    4.00    --  112.00  75.00   7.16   98
 24  \w     79.00 178.00   1.00    4.00    --  112.00  77.00  90.00   99
 25  \w     29.00 109.00   1.00    4.00    --  112.00 -94.00 -30.00   80
 26  \w     79.00 178.00   1.00    4.00    --  112.00  77.00 -90.00   99
 27  \w     57.00 151.00   1.00    4.00    --  112.00 178.00 -30.00   94
 28  \w   -118.00  -9.00   1.00    1.00    --  -41.85 -77.00  90.00  109
 29  \w   -118.00  -9.00   1.00    1.00    --  -41.85 -77.00 120.00  109
 30  \w   -118.00  -9.00   1.00    1.00    --  -41.85 -77.00-180.00  109
 31  \w    -74.00  34.00   1.00    1.00    --  -41.85  77.00 -30.00  108
 32  \w      9.00 118.00   1.00    1.00    --   41.85  77.00 -60.00  109
 33  \w      9.00 118.00   1.00    1.00    --   41.85  77.00  30.00  109
 34  \w     84.00 178.00   1.00    4.00    --  112.00  30.00-180.00   94
 35  \w     86.00 178.00   1.00    4.00    --  112.00  45.00  60.00   92
 36  \w     79.00 178.00   1.00    4.00    --  112.00  77.00-180.00   99
 37  \w     80.00 160.00   1.00    4.00    --  112.00  73.00 117.95   80
 38  \w     86.00 178.00   1.00    4.00    --  112.00  45.00-120.00   92
;
_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      0.0862054000
_diffrn_orient_matrix_UB_12      -0.0703452000
_diffrn_orient_matrix_UB_13      -0.0591656000
_diffrn_orient_matrix_UB_21      -0.1388492000
_diffrn_orient_matrix_UB_22      -0.1163280000
_diffrn_orient_matrix_UB_23      -0.0073124000
_diffrn_orient_matrix_UB_31      -0.1056701000
_diffrn_orient_matrix_UB_32      0.0297429000
_diffrn_orient_matrix_UB_33      -0.0679028000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            32088
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.664
_diffrn_reflns_theta_min         3.993
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.254
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64349
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_description       block
_exptl_crystal_F_000             692
_exptl_crystal_recrystallization_method
'crystallization was induced by gas phase diffusion of n-hexane into a deuterochloroform solution containing the compound as a by-product.'
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.565
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         6679
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0450
_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^)+(0.0795P)^2^+0.4780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1206
_refine_ls_wR_factor_ref         0.1275
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5812
_reflns_number_total             6679
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03044a2.cif
_cod_data_source_block           3dtriclinic
_cod_depositor_comments
'Adding full bibliography for 7701221--7701232.cif.'
_cod_database_code               7701226
_shelx_shelxl_version_number     2018/3
_cell_oxdiff_length_a            8.2514(4)
_cell_oxdiff_length_b            11.6965(5)
_cell_oxdiff_length_c            17.6863(6)
_cell_oxdiff_angle_alpha         101.701(3)
_cell_oxdiff_angle_beta          97.017(3)
_cell_oxdiff_angle_gamma         102.970(4)
_cell_oxdiff_volume              1603.49(11)
_cell_oxdiff_measurement_reflns_used 15424
_shelx_estimated_absorpt_t_min   0.634
_shelx_estimated_absorpt_t_max   0.745
_oxdiff_exptl_absorpt_empirical_full_min 0.481
_oxdiff_exptl_absorpt_empirical_full_max 2.439
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              5477