A N-heterocyclic tetracarbene Pd(ii) moiety containing a Pd(ii)-Pb(ii) bimetallic MOF for three-component cyclotrimerization via benzyne.
Dong, Ying; Li, Yue; Wei, Yong-Liang; Wang, Jian-Cheng; Ma, Jian-Ping; Ji, Jun; Yao, Bing-Jian; Dong, Yu-Bin; Chemical communications (Cambridge, England) 52 (2016) 10505–10508; doi:10.1039/c6cc04570g

data_7124773
_publ_section_title
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 A N-heterocyclic tetracarbene Pd(ii) moiety containing a Pd(ii)-Pb(ii)
 bimetallic MOF for three-component cyclotrimerization via benzyne.
;
_journal_issue                   69
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              10505
_journal_page_last               10508
_journal_paper_doi               10.1039/c6cc04570g
_journal_volume                  52
_journal_year                    2016
_chemical_formula_sum            'C44 H28 Br4 N8 O12 Pb4 Pd'
_chemical_formula_weight         2115.54
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-04-07 deposited with the CCDC.
2016-07-28 downloaded from the CCDC.
;
_cell_angle_alpha                105.216(13)
_cell_angle_beta                 105.376(9)
_cell_angle_gamma                94.884(9)
_cell_formula_units_Z            1
_cell_length_a                   7.634(5)
_cell_length_b                   13.084(8)
_cell_length_c                   14.166(10)
_cell_measurement_reflns_used    1470
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      23.590
_cell_measurement_theta_min      3.066
_cell_volume                     1298.1(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_av_sigmaI/netI    0.1233
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6690
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    16.409
_exptl_absorpt_correction_T_max  0.5598
_exptl_absorpt_correction_T_min  0.1050
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.706
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             958
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         4.474
_refine_diff_density_min         -3.457
_refine_diff_density_rms         0.446
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         4563
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.1032
_refine_ls_R_factor_gt           0.0718
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0798P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1639
_refine_ls_wR_factor_ref         0.1723
_reflns_number_gt                2924
_reflns_number_total             4563
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6cc04570g3.cif
_cod_data_source_block           150513d
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        1298.2(15)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7124773