Crystalline Polymers Based on Dative Boron‒Nitrogen Bonds and the Quest for Porosity
Stephens, Alexander J.; Scopelliti, Rosario; Tirani, Farzaneh Fadaei; Solari, Euro; Severin, Kay; ACS Materials Letters 1 (2019) 3–; doi:10.1021/acsmaterialslett.9b00054

data_4515192
_publ_section_title
;
 Crystalline Polymers Based on Dative Boron--Nitrogen Bonds and the Quest
 for Porosity
;
_journal_issue                   1
_journal_name_full               'ACS Materials Letters'
_journal_page_first              3
_journal_paper_doi               10.1021/acsmaterialslett.9b00054
_journal_volume                  1
_journal_year                    2019
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C69 H48 B4 N4 O8, 2(C6 H4 Cl2)'
_chemical_formula_sum            'C81 H56 B4 Cl4 N4 O8'
_chemical_formula_weight         1398.33
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.50238(13)
_cell_length_b                   21.17437(16)
_cell_length_c                   21.92873(17)
_cell_measurement_reflns_used    24254
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      75.0150
_cell_measurement_theta_min      3.6200
_cell_volume                     6733.85(9)
_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_molecular_graphics    'Mercury 3.10.3 (CCDC, 2018)'
_computing_publication_material  'CIFTab (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2665
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_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    -70.00  30.00   1.00    7.50    --  -43.01  57.00 -60.00  100
  2  \w      6.00  80.00   1.00    7.50    --   43.01 -99.00  90.00   74
  3  \w     23.00  66.00   1.00    7.50    --   43.01-125.00  30.00   43
  4  \w     33.00 113.00   1.00   30.00    --  109.26-111.00  90.00   80
  5  \w     96.00 130.00   1.00   30.00    --  109.26-144.00  68.00   34
  6  \w     63.00 110.00   1.00   30.00    --  109.26-111.00-120.00   47
  7  \w     96.00 129.00   1.00   30.00    --  109.26 -77.00-180.00   33
  8  \w    131.00 176.00   1.00   30.00    --  109.26  30.00 -90.00   45
  9  \w     94.00 163.00   1.00   30.00    --  109.26  30.00-120.00   69
 10  \w     62.00 150.00   1.00   30.00    --  109.26 178.00 -90.00   88
 11  \w    112.00 139.00   1.00   30.00    --  109.26 178.00-120.00   27
 12  \w     70.00  96.00   1.00   30.00    --  109.26 178.00-120.00   26
 13  \w     32.00 160.00   1.00   30.00    --  109.26 -15.00-120.00  128
 14  \w     47.00 124.00   1.00   30.00    --  109.26 -45.00  30.00   77
 15  \w     43.00 137.00   1.00   30.00    --  109.26 -61.00 -90.00   94
 16  \w     39.00 135.00   1.00   30.00    --  109.26 -45.00 150.00   96
 17  \w   -108.00 -18.00   1.00    7.50    --  -43.01 -57.00 150.00   90
 18  \w   -114.00 -88.00   1.00    7.50    --  -43.01 -99.00-150.00   26
 19  \w   -118.00 -80.00   1.00    7.50    --  -43.01 -99.00 -90.00   38
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            23040
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.436
_diffrn_reflns_theta_min         3.694
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.113
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.189
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear intense orange'
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_description       prism
_exptl_crystal_F_000             2888
_exptl_crystal_size_max          0.518
_exptl_crystal_size_mid          0.449
_exptl_crystal_size_min          0.356
_refine_diff_density_max         0.496
_refine_diff_density_min         -0.276
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Flack x determined using 5068 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.341(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1051
_refine_ls_number_reflns         23040
_refine_ls_number_restraints     778
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0666
_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^)+(0.1290P)^2^+1.3654P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1891
_refine_ls_wR_factor_ref         0.1987
_reflns_Friedel_coverage         0.896
_reflns_Friedel_fraction_full    0.975
_reflns_Friedel_fraction_max     0.939
_reflns_number_gt                19830
_reflns_number_total             23040
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tz9b00054_si_001.cif
_cod_data_source_block           ajs-c-001o
_cod_database_code               4515192
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.407
_shelx_estimated_absorpt_t_max   0.520
_shelx_res_checksum              54017
_shelx_hkl_checksum              31771