The synthesis and topochemical polymerization of o-carborane-based diacetylene macrocycles
Fu, Meigui; Yuan, Shuai; Qu, Qi; Yuan, Yaofeng; Lin, Caixia; Geng, Yanhou; New Journal of Chemistry 47 (2023) 21714–21719; doi:10.1039/D3NJ03491G

data_7062795
_publ_section_title
;
 The synthesis and topochemical polymerization of o-carborane-based
 diacetylene macrocycles
;
_journal_issue                   47
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              21714
_journal_page_last               21719
_journal_paper_doi               10.1039/D3NJ03491G
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C40 H44 B20 O4, 1.5[CH2Cl2]'
_chemical_formula_sum            'C41.5 H47 B20 Cl3 O4'
_chemical_formula_weight         932.676
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_audit_creation_date             2023-10-07
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-10-07 deposited with the CCDC.	2023-10-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.082(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.8158(3)
_cell_length_b                   27.3194(6)
_cell_length_c                   9.4186(3)
_cell_measurement_reflns_used    7574
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.2140
_cell_measurement_theta_min      3.2280
_cell_volume                     2560.22(13)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.9961
_diffrn_measured_fraction_theta_max 0.9515
_diffrn_measurement_device_type  'CCD Area Detector'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.9961
_diffrn_reflns_Laue_measured_fraction_max 0.9515
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            18953
_diffrn_reflns_point_group_measured_fraction_full 0.9961
_diffrn_reflns_point_group_measured_fraction_max 0.9515
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         76.79
_diffrn_reflns_theta_min         4.44
_exptl_absorpt_coefficient_mu    1.916
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85412
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_description       needle
_exptl_crystal_F_000             962.693
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.2576
_refine_diff_density_min         -0.3195
_refine_diff_density_rms         0.0660
_refine_ls_d_res_high            0.7919
_refine_ls_d_res_low             9.9499
_refine_ls_goodness_of_fit_ref   1.0367
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    42
_refine_ls_number_parameters     289
_refine_ls_number_reflns         5137
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0367
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0686
_refine_ls_shift/su_max          0.0017
_refine_ls_shift/su_mean         0.0002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0489P)^2^+3.0477P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1669
_refine_ls_wR_factor_ref         0.1735
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -13
_reflns_limit_k_max              34
_reflns_limit_k_min              0
_reflns_limit_l_max              11
_reflns_limit_l_min              0
_reflns_number_gt                4476
_reflns_number_total             5137
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3nj03491g2.cif
_cod_data_source_block           2-2_auto_sq
_cod_depositor_comments
'Adding full bibliography for 7062794--7062795.cif.'
_cod_database_code               7062795
_olex2_refinement_description
;
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 138 electrons were 
found in a volume of 482\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 1.5[CH2Cl2] per Formula Unit 
which account for 126 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_refine_details
;
Refinement using NoSpherA2, an implementation of
NOn-SPHERical Atom-form-factors in Olex2.
Please cite:
F. Kleemiss et al. Chem. Sci. DOI 10.1039/D0SC05526C - 2021
NoSpherA2 implementation of HAR makes use of
tailor-made aspherical atomic form factors calculated
on-the-fly from a Hirshfeld-partitioned electron density (ED) - not from
spherical-atom form factors.

The ED is calculated from a gaussian basis set single determinant SCF
wavefunction - either Hartree-Fock or DFT using selected funtionals
 - for a fragment of the crystal.
This fragment can be embedded in an electrostatic crystal field by employing cluster charges
or modelled using implicit solvation models, depending on the software used.
The following options were used:
   SOFTWARE:       ORCA 5.0
   PARTITIONING:   NoSpherA2
   INT ACCURACY:   Normal
   METHOD:         R2SCAN
   BASIS SET:      def2-TZVP
   CHARGE:         0
   MULTIPLICITY:   1
   DATE:           2023-09-21_14-35-22
;
_olex2_submission_special_instructions 'No special instructions were received'