A Pd4Br4 macrocycle trapped by cocrystallization from a highly dynamic equilibrium of η(3)-cycloheptatrienide complexes.
Jandl, C.; Stegbauer, S.; Pöthig, A; Acta crystallographica. Section C, Structural chemistry 72 (2016) 509–513; doi:10.1107/S2053229616008275

data_2311857
_publ_section_title
;
 A Pd4Br4 macrocycle trapped by cocrystallization from a highly dynamic
 equilibrium of \h(3)-cycloheptatrienide complexes.
;
_journal_coeditor_code           FP3030
_journal_issue                   'Pt 7'
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_page_first              509
_journal_page_last               513
_journal_paper_doi               10.1107/S2053229616008275
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac
'[Pd4 Br4 (C22 H26 N2)4 ] [Pd2 Br2 (C22 H26 N2)2]2 (B F4)8, 8C H2 Cl2'
_chemical_formula_moiety
'C88 H104 Br4 N8 Pd4 4+, 2(C44 H52 Br2 N4 Pd2 2+), 8(B F4 -), 8(C H2 Cl2)'
_chemical_formula_sum            'C184 H224 B8 Br8 Cl16 F32 N16 Pd8'
_chemical_formula_weight         5411.87
_chemical_name_systematic
;Bis[di-\m-bromido-bis({\h^3^-[3-(2,6-diisopropylphenyl)imidazolium-1-yl]cycloheptatrienido}palladium(II))]
<i>cyclo</i>-tetra-\m-bromido-tetrakis({\h^3^-[3-(2,6-diisopropylphenyl)imidazolium-1-yl]cycloheptatrienido}palladium(II)) octakis(tetrafluoroborate)
dichloromethane octasolvate
;
_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_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                78.2025(13)
_cell_angle_beta                 82.7526(14)
_cell_angle_gamma                85.7404(12)
_cell_formula_units_Z            1
_cell_length_a                   15.7247(4)
_cell_length_b                   18.8101(5)
_cell_length_c                   19.1726(5)
_cell_measurement_reflns_used    9553
_cell_measurement_temperature    123
_cell_measurement_theta_max      28.3120
_cell_measurement_theta_min      2.1845
_cell_volume                     5499.9(2)
_computing_cell_refinement
;
SAINT (Bruker, 2012)
;
_computing_data_collection
;
APEX2 (Bruker, 2013)
;
_computing_data_reduction
;
SAINT (Bruker, 2012)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>, 2008)
;
_computing_publication_material
;
PLATON (Spek, 2009), enCIFer (Allen <i>et al.</i>, 2004)
and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015) and
SHELXLE (H\"ubschle <i>et al.</i>, 2011)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       ' \k-geometry diffractometer '
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_radiation_monochromator  'MONTEL optic'
_diffrn_radiation_source         'rotating anode FR591'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            127005
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    2.364
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6567
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2012)
;
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       rhombus
_exptl_crystal_F_000             2688
_exptl_crystal_size_max          0.295
_exptl_crystal_size_mid          0.134
_exptl_crystal_size_min          0.071
_refine_diff_density_max         0.767
_refine_diff_density_min         -1.568
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1343
_refine_ls_number_reflns         22490
_refine_ls_number_restraints     279
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0300
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'W=1/[\S^2^(FO^2^)+(0.0387P)^2^+7.2466P] WHERE P=(FO^2^+2FC^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0748
_refine_ls_wR_factor_ref         0.0798
_reflns_number_gt                18569
_reflns_number_total             22490
_reflns_threshold_expression     i>2\s(i)
_cod_data_source_file            fp3030sup1.cif
_cod_data_source_block           I
_cod_database_code               2311857
_shelx_hkl_checksum              26469
_shelx_res_checksum              9296
_shelxl_version_number           2014/6