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_7701230
_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 O8 P'
_chemical_formula_weight         646.60
_chemical_name_systematic
(3,3??,5,5??-Tetramethoxycarbonyl-1,1?:3?,1??-terphen-2?-yl)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                84.946(2)
_cell_angle_beta                 89.978(2)
_cell_angle_gamma                83.828(2)
_cell_formula_units_Z            4
_cell_length_a                   10.0692(2)
_cell_length_b                   14.1456(4)
_cell_length_c                   22.7621(6)
_cell_measurement_reflns_used    20707
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.0040
_cell_measurement_theta_min      3.1590
_cell_volume                     3210.66(14)
_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 5.2063
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.975
_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    -77.00 -27.00   1.00   32.50    --  -15.74 131.00 -91.65   50
  2  \w    -60.00  42.00   1.00   32.50    --   15.74 -38.00-120.00  102
  3  \w    -11.00  92.00   1.00   32.50    --   15.74  38.00 -30.00  103
  4  \w    -11.00  92.00   1.00   32.50    --   15.74  38.00  60.00  103
  5  \w    -58.00  45.00   1.00   32.50    --   15.74 -57.00  30.00  103
  6  \w    -63.00  49.00   1.00   32.50    --   15.74 -77.00 150.00  112
  7  \w    -18.00  94.00   1.00   32.50    --   15.74  77.00 150.00  112
  8  \w    -20.00  26.00   1.00   32.50    --  -15.74 -99.00-180.00   46
  9  \w   -104.00 -55.00   1.00   32.50    --  -15.74 178.00-150.00   49
 10  \w    -76.00 -27.00   1.00   32.50    --  -15.74 129.00  42.55   49
 11  \w    -20.00  26.00   1.00   32.50    --  -15.74 -99.00 -60.00   46
 12  \w    -77.00 -27.00   1.00   32.50    --  -15.74 131.00 110.50   50
 13  \w    -87.00 -37.00   1.00   32.50    --  -15.74 149.00 165.00   50
 14  \w    -77.00 -27.00   1.00   32.50    --  -15.74 131.00 -28.38   50
 15  \w    -93.00 -39.00   1.00   32.50    --  -15.74 154.00 164.58   54
 16  \w     35.00 106.00   1.00   32.50    --   15.74 178.00  30.00   71
;
_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      -0.0355836000
_diffrn_orient_matrix_UB_12      0.0250403000
_diffrn_orient_matrix_UB_13      -0.0245086000
_diffrn_orient_matrix_UB_21      -0.0494154000
_diffrn_orient_matrix_UB_22      0.0189301000
_diffrn_orient_matrix_UB_23      0.0192487000
_diffrn_orient_matrix_UB_31      0.0362286000
_diffrn_orient_matrix_UB_32      0.0397297000
_diffrn_orient_matrix_UB_33      0.0027441000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0730
_diffrn_reflns_av_unetI/netI     0.0587
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            100462
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_min         2.822
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.140
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57817
_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    1.338
_exptl_crystal_description       rod
_exptl_crystal_F_000             1352
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol/tetrahydrofuran'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.062
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     855
_refine_ls_number_reflns         18240
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0988
_refine_ls_R_factor_gt           0.0732
_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^)+(0.0582P)^2^+4.8547P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1677
_refine_ls_wR_factor_ref         0.1809
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13886
_reflns_number_total             18240
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03044a2.cif
_cod_data_source_block           3e
_cod_depositor_comments
'Adding full bibliography for 7701221--7701232.cif.'
_cod_database_code               7701230
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.953
_shelx_estimated_absorpt_t_max   0.993
_oxdiff_exptl_absorpt_empirical_full_min 0.561
_oxdiff_exptl_absorpt_empirical_full_max 1.551
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_theta     28.22
_reflns_odcompleteness_iscentric 1
_shelx_res_checksum              5881