Topologically diverse polycyclic aromatic hydrocarbons from pericyclic reactions with polyaromatic phospholes
Mokrai, Réka; Szűcs, Rózsa; Duffy, Matthew P.; Dorcet, Vincent; Roisnel, Thierry; Benkő, Zoltán; Nyulászi, László; Bouit, Pierre-Antoine; Hissler, Muriel; New Journal of Chemistry 45 (2021) 8118–8124; doi:10.1039/D1NJ01194D

data_1561780
_publ_section_title
;
 Topologically diverse polycyclic aromatic hydrocarbons from pericyclic
 reactions with polyaromatic phospholes
;
_journal_issue                   18
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              8118
_journal_page_last               8124
_journal_paper_doi               10.1039/D1NJ01194D
_journal_volume                  45
_journal_year                    2021
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C17 H15 Cu N4 O3, 3.5(H2 O)'
_chemical_formula_structural     'C17 H15 Cu N4 O3, 3.5(H2 O)'
_chemical_formula_sum            'C17 H22 Cu N4 O6.5'
_chemical_formula_weight         449.92
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/cc6m9qt
_audit_conform_dict_location     ftp://ftp.iucr.org/cifdics/cif_core2.1beta.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1beta3
_audit_creation_date             1999-09-13T16:37:49-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2002-11-11 deposited with the CCDC.	2021-04-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.440(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.984(8)
_cell_length_b                   17.472(3)
_cell_length_c                   12.480(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_measurement_wavelength     0.71073
_cell_volume                     1932.4(18)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_orient_matrix_type
;
x-axis points to radiation source
the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      -0.29531E-1
_diffrn_orient_matrix_UB_12      0.01069
_diffrn_orient_matrix_UB_13      -0.79361E-1
_diffrn_orient_matrix_UB_21      0.11211E-1
_diffrn_orient_matrix_UB_22      0.56169E-1
_diffrn_orient_matrix_UB_23      0.14627E-1
_diffrn_orient_matrix_UB_31      0.10831
_diffrn_orient_matrix_UB_32      -0.2902E-2
_diffrn_orient_matrix_UB_33      -0.9274E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0641
_diffrn_reflns_av_sigmaI/netI    0.1781
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6067
_diffrn_reflns_theta_full        30.42
_diffrn_reflns_theta_max         30.42
_diffrn_reflns_theta_min         2.3
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 79
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.175
_exptl_absorpt_correction_T_max  0.9328
_exptl_absorpt_correction_T_min  0.5539
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
Number of psi-scan sets used was   7
Theta correction was applied.
Averaged transmission function was used.
No Fourier smoothing was applied.
;
_exptl_crystal_colour            -
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.416
_refine_diff_density_min         -0.702
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.001(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     570
_refine_ls_number_reflns         5763
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      0.97
_refine_ls_R_factor_all          0.1886
_refine_ls_R_factor_gt           0.0427
_refine_ls_shift/su_max          0.095
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0927
_refine_ls_wR_factor_ref         0.1204
_reflns_number_gt                2996
_reflns_number_total             5763
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d1nj01194d2.cif
_cod_data_source_block           pm38
_cod_depositor_comments
;
Adding full bibliography for 1561780--1561785.cif.

2022-04-28
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C34 H44 Cu2 N8 O13'
_cod_original_formula_weight         899.85
_cod_original_formula_moiety         'C34 H44 Cu2 N8 O13'
_cod_original_formula_units_Z            2
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1561780
_exptl_absorpt_factor_mur        0.192
_exptl_absorpt_correction_t_ave  0.7851
_diffrn_standards_decay_corr_max 1
_diffrn_standards_decay_corr_min 1