One-step synthesis of a cyclic 2,17-dioxo[3,3](4,4') biphenylophane and first preparation of a microporous polymer network from a macrocyclic precursor by cyclotrimerization
Suman Kalyan Samanta; Eduard Preis; Christian W. Lehmann; Richard Goddard; Saientan Bag; Prabal K. Maiti; Gunther Brunklaus; Ullrich Scherf; Chem.Commun. 51 (2015) 9046–; doi:10.1039/C5cc01654A

data_7117175
_publ_section_title
;
 One-step synthesis of a cyclic 2,17-dioxo[3,3](4,4') biphenylophane and
 first preparation of a microporous polymer network from a macrocyclic
 precursor by cyclotrimerization
;
_journal_name_full               Chem.Commun.
_journal_page_first              9046
_journal_paper_doi               10.1039/C5cc01654A
_journal_volume                  51
_journal_year                    2015
_chemical_compound_source        unknown
_chemical_formula_moiety         'C30 H24 O2'
_chemical_formula_sum            'C30 H24 O2'
_chemical_formula_weight         416.49
_chemical_name_systematic
; 
2,17-Dioxo[3,3](4,4')biphenylophane
;
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                EMC-EA-200_8996_ANKA56_8837_MC
_audit_creation_date             2015-02-18
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-02-18 deposited with the CCDC.
2015-04-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.254(11)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   31.067(15)
_cell_length_b                   13.835(6)
_cell_length_c                   15.670(7)
_cell_measurement_reflns_used    9793
_cell_measurement_temperature    150
_cell_measurement_theta_max      32.383
_cell_measurement_theta_min      2.3435
_cell_volume                     6724(5)
_computing_cell_refinement       'SAINT software (Bruker AXS, 2004)'
_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'SAINT software (Bruker AXS, 2004)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 2005)'
_computing_structure_refinement  'SHELXL-2014/7 (G. M. Sheldrick, 1993-2014)'
_computing_structure_solution    'SHELXS-97 (G. M. Sheldrick, 2014)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 66.67
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_device_type  'Bruker-AXS Smart APEX-II'
_diffrn_measurement_method       'CCD \f- and \w-scans'
_diffrn_radiation_monochromator  Si(111)
_diffrn_radiation_source         'Synchrotron ANKA, FZK, Karlsruhe'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.80000
_diffrn_reflns_av_unetI/netI     0.1225
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            72812
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_theta_full        28.685
_diffrn_reflns_theta_max         32.051
_diffrn_reflns_theta_min         1.478
_exptl_absorpt_coefficient_mu    0.097
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.452782
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS (Bruker AXS, v. 2012/1)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       needle
_exptl_crystal_F_000             2640
_exptl_crystal_size_max          0.440
_exptl_crystal_size_mid          0.016
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.448
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.089
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         72812
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1448
_refine_ls_R_factor_gt           0.0858
_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^)+(0.0283P)^2^+7.9824P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1739
_refine_ls_wR_factor_ref         0.1979
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                43956
_reflns_number_total             72812
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc01654a2.cif
_cod_data_source_block           8996
_cod_database_code               7117175
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.959
_shelx_estimated_absorpt_t_max   0.999
_shelx_res_checksum              64085
_shelx_hkl_checksum              43478