Tailoring Diradicaloid Properties of Expanded Isophlorinoids with Systematic Core-Modification
Ambhore, Madan Digambar; SHUKLA, PRAGATI; Gonnade, Rajesh G.; Anand, Venkataramanarao Govindan; Chemical Communications  (2022) –; doi:10.1039/D2CC02970G

data_7130325
_publ_section_title
;
 Tailoring Diradicaloid Properties of Expanded Isophlorinoids with
 Systematic Core-Modification
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC02970G
_journal_year                    2022
_chemical_formula_moiety         'C74 H26 F20 O4 S4, 4 (C H CL3)'
_chemical_formula_sum            'C78 H30 Cl12 F20 O4 S4'
_chemical_formula_weight         1964.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-06-21 deposited with the CCDC.	2022-07-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.851(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.994(3)
_cell_length_b                   28.344(4)
_cell_length_c                   11.9777(15)
_cell_measurement_reflns_used    9859
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.98
_cell_measurement_theta_min      2.32
_cell_volume                     8071.2(18)
_computing_cell_refinement       'SAINT (Bruker, 2016)'
_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_data_reduction        'SAINT (Bruker, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CMOS-Photon 100'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'D8 VENTURE APEX'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1223
_diffrn_reflns_av_unetI/netI     0.0791
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            107896
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.480
_diffrn_reflns_theta_min         2.320
_diffrn_source                   'micro-focus sealed tube'
_diffrn_source_type              micro-focus
_exptl_absorpt_coefficient_mu    0.612
_exptl_absorpt_correction_T_max  0.0962
_exptl_absorpt_correction_T_min  0.0682
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS(Bruker, 2016)'
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             3912
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.036
_platon_squeeze_details
;
PLATON/SQUEEZE was used to correct the diffraction data for the 
contribution from disordered lattice solvent (chloroform) molecules. 
The solvent accessible void volume per unit cell was 2649 A3 (33%) 
and Electron Count/unit Cell was 890 e/A-3, estimated by PLATON. 
This electron count corresponds to four disordered chloroform molecules 
present in the unit cell. However, they have been included in
SFAC and UNIT instructions to get the correct molecular formula 
of the asymmetruc unit, formula weight, crystal density and F(000). 
;
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         10144
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1091
_refine_ls_R_factor_gt           0.0595
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0593P)^2^+8.6178P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1234
_refine_ls_wR_factor_ref         0.1383
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6320
_reflns_number_total             10144
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02970g2.cif
_cod_data_source_block           7
_cod_original_cell_volume        8071.2(17)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7130325
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.857
_shelx_estimated_absorpt_t_max   0.978
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              27951
_shelx_hkl_checksum              8954
_shelx_fab_checksum              38648