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_7701221
_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            'C18 H13 Cl2 P'
_chemical_formula_weight         331.15
_chemical_name_systematic        (2,6-Dichlorophenyl)diphenylphosphane
_chemical_properties_physical    Air-sensitive
_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
_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                105.361(3)
_cell_angle_beta                 104.778(3)
_cell_angle_gamma                110.456(3)
_cell_formula_units_Z            2
_cell_length_a                   8.2413(3)
_cell_length_b                   9.8910(3)
_cell_length_c                   11.4287(3)
_cell_measurement_reflns_used    12940
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.1160
_cell_measurement_theta_min      4.3240
_cell_volume                     776.87(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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 5.2063
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.986
_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    --  -42.35 125.00 120.00   94
  2  \w   -117.00 -18.00   1.00    1.00    --  -42.35 -38.00 -90.00   99
  3  \w    -67.00  32.00   1.00    1.00    --  -42.35  38.00  90.00   99
  4  \w     36.00 140.00   1.00    1.00    --  112.00 -30.00  60.00  104
  5  \w     29.00 109.00   1.00    1.00    --  112.00 -94.00 120.00   80
  6  \w     83.00 178.00   1.00    1.00    --  112.00  61.00  90.00   95
  7  \w     36.00 116.00   1.00    1.00    --  112.00-111.00 -30.00   80
  8  \w     36.00 116.00   1.00    1.00    --  112.00-111.00-120.00   80
  9  \w     57.00 151.00   1.00    1.00    --  112.00 178.00 -30.00   94
 10  \w     36.00 116.00   1.00    1.00    --  112.00-111.00  60.00   80
 11  \w     30.00 165.00   1.00    1.00    --  112.00 -15.00 -90.00  135
 12  \w     40.00 141.00   1.00    1.00    --  112.00 -61.00 -60.00  101
 13  \w     29.00 109.00   1.00    1.00    --  112.00 -94.00-180.00   80
 14  \w     57.00 151.00   1.00    1.00    --  112.00 178.00   0.00   94
 15  \w   -119.00 -10.00   1.00    1.00    --  -42.35 -77.00   0.00  109
 16  \w   -115.00 -14.00   1.00    1.00    --  -42.35 -57.00 150.00  101
 17  \w   -119.00 -10.00   1.00    1.00    --  -42.35 -77.00  90.00  109
 18  \w      1.00  83.00   1.00    1.00    --   42.35 -99.00 -60.00   82
 19  \w     83.00 178.00   1.00    1.00    --  112.00  61.00  60.00   95
 20  \w     83.00 178.00   1.00    1.00    --  112.00  61.00  30.00   95
 21  \w     59.00 178.00   1.00    1.00    --  112.00  15.00-150.00  119
 22  \w     83.00 178.00   1.00    1.00    --  112.00  61.00-150.00   95
 23  \w     59.00 178.00   1.00    1.00    --  112.00  15.00   0.00  119
 24  \w     83.00 178.00   1.00    1.00    --  112.00  61.00 -90.00   95
 25  \w     83.00 178.00   1.00    1.00    --  112.00  61.00   0.00   95
 26  \w     83.00 178.00   1.00    1.00    --  112.00  61.00-180.00   95
 27  \w     83.00 178.00   1.00    1.00    --  112.00  61.00 120.00   95
 28  \w     79.00 178.00   1.00    1.00    --  112.00  77.00 -60.00   99
 29  \w     83.00 178.00   1.00    1.00    --  112.00  61.00 150.00   95
 30  \w     83.00 178.00   1.00    1.00    --  112.00  61.00-120.00   95
 31  \w   -119.00 -10.00   1.00    1.00    --  -42.35 -77.00 -90.00  109
 32  \w   -119.00 -10.00   1.00    1.00    --  -42.35 -77.00-180.00  109
 33  \w   -117.00 -18.00   1.00    1.00    --  -42.35 -38.00  90.00   99
 34  \w   -125.00 -78.00   1.00    1.00    --  -42.35 -87.00  59.00   47
 35  \w     79.00 118.00   1.00    1.00    --  112.00  77.00 -30.00   39
;
_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      -0.0409339000
_diffrn_orient_matrix_UB_12      0.1106575000
_diffrn_orient_matrix_UB_13      -0.0625941000
_diffrn_orient_matrix_UB_21      0.1597415000
_diffrn_orient_matrix_UB_22      0.1426153000
_diffrn_orient_matrix_UB_23      0.1208906000
_diffrn_orient_matrix_UB_31      0.1397526000
_diffrn_orient_matrix_UB_32      -0.0056523000
_diffrn_orient_matrix_UB_33      -0.0663751000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15427
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.453
_diffrn_reflns_theta_min         4.346
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.631
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77706
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_description       block
_exptl_crystal_F_000             340
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: ethanol'
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.350
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3228
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0289
_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^)+(0.0424P)^2^+0.4588P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0762
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3145
_reflns_number_total             3228
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03044a2.cif
_cod_data_source_block           2d
_cod_depositor_comments
'Adding full bibliography for 7701221--7701232.cif.'
_cod_original_cell_volume        776.87(5)
_cod_database_code               7701221
_shelx_shelxl_version_number     2018/3
_cell_oxdiff_length_a            8.2413(3)
_cell_oxdiff_length_b            9.8910(3)
_cell_oxdiff_length_c            11.4287(3)
_cell_oxdiff_angle_alpha         105.361(3)
_cell_oxdiff_angle_beta          104.778(3)
_cell_oxdiff_angle_gamma         110.456(3)
_cell_oxdiff_volume              776.87(4)
_cell_oxdiff_measurement_reflns_used 12940
_shelx_estimated_absorpt_t_min   0.265
_shelx_estimated_absorpt_t_max   0.443
_oxdiff_exptl_absorpt_empirical_full_min 0.630
_oxdiff_exptl_absorpt_empirical_full_max 4.516
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              72516