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_4515193
_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_formula_moiety         'C73 H52 B4 N8 O8'
_chemical_formula_sum            'C73 H52 B4 N8 O8'
_chemical_formula_weight         1212.46
_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     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                87.084(5)
_cell_angle_beta                 75.549(5)
_cell_angle_gamma                72.540(6)
_cell_formula_units_Z            2
_cell_length_a                   12.1125(8)
_cell_length_b                   15.6299(10)
_cell_length_c                   23.3077(12)
_cell_measurement_reflns_used    7904
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      73.0660
_cell_measurement_theta_min      3.8980
_cell_volume                     4074.7(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Mercury 4.0.0 (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 0.987
_diffrn_measured_fraction_theta_max 0.947
_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   -109.00 -19.00   1.00    8.96    --  -43.01 -57.00  30.00   90
  2  \w    -89.00 -40.00   1.00    8.96    --  -43.01 125.00-120.00   49
  3  \w   -118.00 -84.00   1.00    8.96    --  -43.01 -99.00  90.00   34
  4  \w    -69.00  30.00   1.00    8.96    --  -43.01  57.00-180.00   99
  5  \w    -66.00  12.00   1.00    8.96    --  -43.01  37.00   0.00   78
  6  \w     81.00 108.00   1.00   35.84    --  105.68 -94.00 120.00   27
  7  \w     24.00 109.00   1.00   35.84    --  105.68 -94.00 -30.00   85
  8  \w     40.00 134.00   1.00   35.84    --  105.68 -30.00 -90.00   94
  9  \w    138.00 167.00   1.00   35.84    --  105.68  61.00 -90.00   29
 10  \w    108.00 176.00   1.00   35.84    --  105.68 125.00 -30.00   68
 11  \w    140.00 165.00   1.00   35.84    --  105.68 125.00 120.00   25
 12  \w     36.00  63.00   1.00   35.84    --  105.68 -94.00 120.00   27
 13  \w     92.00 178.00   1.00   35.84    --  105.68  30.00  90.00   86
 14  \w    113.00 171.00   1.00   35.84    --  105.68 125.00  30.00   58
 15  \w     96.00 151.00   1.00   35.84    --  105.68 126.00   6.00   55
 16  \w     38.00 109.00   1.00   35.84    --  105.68 -94.00  60.00   71
 17  \w     67.00 144.00   1.00   35.84    --  105.68  15.00-150.00   77
 18  \w     90.00 118.00   1.00   35.84    --  105.68-125.00 -60.00   28
 19  \w     34.00 129.00   1.00   35.84    --  105.68 -61.00  60.00   95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, 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_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            29544
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.258
_diffrn_reflns_theta_min         3.511
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.519
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.125
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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 pale colourless'
_exptl_crystal_density_diffrn    0.988
_exptl_crystal_description       plate
_exptl_crystal_F_000             1260
_exptl_crystal_size_max          0.511
_exptl_crystal_size_mid          0.444
_exptl_crystal_size_min          0.234
_refine_diff_density_max         0.676
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.600
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     826
_refine_ls_number_reflns         15745
_refine_ls_number_restraints     888
_refine_ls_restrained_S_all      1.584
_refine_ls_R_factor_all          0.1516
_refine_ls_R_factor_gt           0.1298
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4025
_refine_ls_wR_factor_ref         0.4293
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11021
_reflns_number_total             15745
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tz9b00054_si_002.cif
_cod_data_source_block           ajs-c-040e
_cod_original_cell_volume        4074.7(4)
_cod_database_code               4515193
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.777
_shelx_estimated_absorpt_t_max   0.888
_shelx_res_checksum              38925
_shelx_hkl_checksum              51246
_shelx_fab_checksum              42539