Synthesis of an adj-Dicarbaporphyrin and the Formation of an Unprecedented Tripalladium Sandwich Complex.
Abusalim, Deyaa I.; Ferrence, Gregory M.; Lash, Timothy D.; Journal of the American Chemical Society 136 (2014) 6763–6772; doi:10.1021/ja502795x

data_4121737
_publ_section_title
;
 Synthesis of an adj-Dicarbaporphyrin and the Formation of an
 Unprecedented Tripalladium Sandwich Complex.
;
_journal_issue                   18
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6763
_journal_page_last               6772
_journal_paper_doi               10.1021/ja502795x
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C72  H56  N4  Pd3, C D Cl3'
_chemical_formula_sum            'C73 H56 Cl3 D N4 Pd3'
_chemical_formula_weight         1416.78
_chemical_name_systematic
;
Bis(\m2-\h5-13,17-Diethyl-12,18-dimethyldibenzo[b,g]-21,22-dicarbaporphyrinato)-dipalladium(ii)-palladium(iv)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-03-13T16:08:37-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                101.888(3)
_cell_angle_beta                 112.316(3)
_cell_angle_gamma                98.620(3)
_cell_formula_units_Z            2
_cell_length_a                   13.5576(6)
_cell_length_b                   13.8032(6)
_cell_length_c                   16.9833(7)
_cell_measurement_reflns_used    9952
_cell_measurement_temperature    80(2)
_cell_measurement_theta_max      27.05
_cell_measurement_theta_min      2.25
_cell_volume                     2784.3(2)
_computing_cell_refinement       'APEX2 & SAINT (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2013)'
_computing_data_reduction        SAINT
_computing_molecular_graphics
;
<i>Ortep-3</i> for Windows (Farrugia, 2012) and <i>Mercury CSD</i> (Macrae et
 al., 2008)
;
_computing_publication_material
;
        <i>WinGX</i> (Farrugia, 2012) and <i>publCIF</i> (Westrip, 2010)
;
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      80(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
A total of 3672 frames were collected.  The total 
exposure time was 183.60 hours.
;
_diffrn_measurement_device_type  'Bruker APEX-II CCD diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1232
_diffrn_reflns_av_unetI/netI     0.0802
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_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            70681
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         1.353
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.154
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5863
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 v2013.2-0 (Bruker, 2013)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.69
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.015
_refine_diff_density_max         4.799
_refine_diff_density_min         -1.317
_refine_diff_density_rms         0.207
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     752
_refine_ls_number_reflns         10936
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.1103
_refine_ls_R_factor_gt           0.0648
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0644P)^2^+37.4552P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1777
_reflns_number_gt                7485
_reflns_number_total             10936
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja502795x_si_001.cif
_cod_data_source_block           gmf14002
_cod_depositor_comments          'Adding full bibliography for 4121737.cif.'
_cod_database_code               4121737
_shelxl_version_number           2012