Synthesis and crystallographic, spectroscopic and computational characterization of 3,3',4,4'-substituted biphenyls: effects of O<i>R</i> substituents on the intra-ring torsion angle
Vadra, Nahir; Suarez, Sebastian A.; Slep, Leonardo D.; Manzano, Veronica E.; Halac, Emilia B.; Baggio, Ricardo F.; Cukiernik, Fabio D.; Acta Crystallographica Section B 76 (2020) –; doi:10.1107/S2052520620004102

data_2108607
_publ_section_title
;
 Synthesis and crystallographic, spectroscopic and computational
 characterization of 3,3',4,4'-substituted biphenyls: effects of O<i>R</i>
 substituents on the intra-ring torsion angle
;
_journal_coeditor_code           LO5065SUP1
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520620004102
_journal_volume                  76
_journal_year                    2020
_chemical_formula_moiety         'C36 H58 O4'
_chemical_formula_sum            'C36 H58 O4'
_chemical_formula_weight         554.82
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2019-11-19 # Formatted by publCIF

;
_cell_angle_alpha                90
_cell_angle_beta                 96.221(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   22.486(2)
_cell_length_b                   8.8585(9)
_cell_length_c                   8.3874(8)
_cell_measurement_reflns_used    8395
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.19
_cell_measurement_theta_min      2.47
_cell_volume                     1660.9(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL   (Sheldrick, 2008)'
_computing_publication_material  'SHELXL-2018, PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL-2018 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.881
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0836
_diffrn_reflns_av_unetI/netI     0.0694
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.881
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            26569
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.881
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.599
_diffrn_reflns_theta_min         2.473
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SAINT'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.109
_exptl_crystal_description       fragment
_exptl_crystal_F_000             612
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.252
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.254
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         4907
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.254
_refine_ls_R_factor_all          0.1083
_refine_ls_R_factor_gt           0.0685
_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^)+(0.0362P)^2^+0.4066P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1330
_refine_ls_wR_factor_ref         0.1432
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3347
_reflns_number_total             4907
_reflns_threshold_expression     'I > 2\s(I)'
_publcif_datablock.id            {47ede442-4831-4e11-8b32-c25b40e29279}
_cod_data_source_file            lo5065sup1.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_primary' value 'direct methods' was
changed to 'direct'.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        1660.8(3)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2108607
_cod_database_fobs_code          2108607
_shelx_shelxl_version_number     2018/1
_shelx_res_checksum              83111
_shelx_hkl_checksum              65509