Design of solvatomorphic structures based on a polyboronated tetraphenyladamantane molecular tecton
Drapała, Jakub; Marek-Urban, Paulina H.; Klimkowski, Piotr; Urbanowicz, Karolina A.; Gontarczyk, Krzysztof; Woźniak, Krzysztof; Luliński, Sergiusz; Durka, Krzysztof; CrystEngComm 23 (2021) 8169–8182; doi:10.1039/D1CE01297E

data_1565079
_publ_section_title
;
 Design of solvatomorphic structures based on a polyboronated
 tetraphenyladamantane molecular tecton
;
_journal_issue                   46
_journal_name_full               CrystEngComm
_journal_page_first              8169
_journal_page_last               8182
_journal_paper_doi               10.1039/D1CE01297E
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C34 H36 B4 O8, 2(C4 H8 O2), H2 O'
_chemical_formula_sum            'C42 H54 B4 O13'
_chemical_formula_weight         810.09
_chemical_name_systematic
;
 tetrakis(4-dihydroxyborylphenyl)adamantane dioxane disolvate water monosolvate
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2021-09-21 deposited with the CCDC.	2021-10-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.4201(7)
_cell_length_b                   17.4201(7)
_cell_length_c                   26.248(3)
_cell_measurement_reflns_used    1559
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      40.0560
_cell_measurement_theta_min      2.9670
_cell_volume                     7965.2(10)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2195
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.337
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 0.337
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            4974
_diffrn_reflns_point_group_measured_fraction_full 0.337
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         40.349
_diffrn_reflns_theta_min         3.045
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.796
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.884
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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            colourless
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_description       shapeless
_exptl_crystal_F_000             3440
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeOH, H2O, Dioxane'
_exptl_crystal_size_max          0.151
_exptl_crystal_size_mid          0.084
_exptl_crystal_size_min          0.077
_refine_diff_density_max         0.477
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.670
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         1222
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.666
_refine_ls_R_factor_all          0.1270
_refine_ls_R_factor_gt           0.1118
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.004
_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          0.3483
_refine_ls_wR_factor_ref         0.3637
_reflns_Friedel_coverage         0.000
_reflns_number_gt                982
_reflns_number_total             1222
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01297e3.cif
_cod_data_source_block           1-Diox-W
_cod_depositor_comments
'Adding full bibliography for 1565076--1565082.cif.'
_cod_original_cell_volume        7965.2(12)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               1565079
_oxdiff_exptl_absorpt_empirical_full_min 0.795
_oxdiff_exptl_absorpt_empirical_full_max 1.571
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelxl_version_number           2013-4
_shelx_res_checksum              51465
_shelx_hkl_checksum              12515