Synthesis of a flexible macrocyclic tetraimidazolium salt-precursor for a tetracarbene ligand with metal dependent coordination modes.
Schulte To Brinke, Christian; Ekkehardt Hahn, F.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 14315–14322; doi:10.1039/c5dt02115d

data_7035704
_publ_section_title
;
 Synthesis of a flexible macrocyclic tetraimidazolium salt-precursor for a
 tetracarbene ligand with metal dependent coordination modes.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14315
_journal_page_last               14322
_journal_paper_doi               10.1039/c5dt02115d
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C36 H40 N8 Pd, 2(F6 P), C2 H3 N'
_chemical_formula_sum            'C38 H43 F12 N9 P2 Pd'
_chemical_formula_weight         1022.15
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_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
;
2015-06-01 deposited with the CCDC.
2015-07-08 downloaded from the CCDC.
;
_cell_angle_alpha                92.8700(10)
_cell_angle_beta                 99.6370(10)
_cell_angle_gamma                112.9970(10)
_cell_formula_units_Z            2
_cell_length_a                   12.0953(5)
_cell_length_b                   12.4132(5)
_cell_length_c                   15.6467(7)
_cell_measurement_reflns_used    10997
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      30.118
_cell_measurement_theta_min      2.3165
_cell_volume                     2114.67(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 80
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'Omega and Phi 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  0.0198
_diffrn_reflns_av_sigmaI/netI    0.0315
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25199
_diffrn_reflns_theta_full        30.15
_diffrn_reflns_theta_max         30.15
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    0.609
_exptl_absorpt_correction_T_max  0.9820
_exptl_absorpt_correction_T_min  0.9250
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Multi-scan correction included in APEX2 package (Bruker AXS, 2012)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.296
_refine_diff_density_min         -0.941
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     596
_refine_ls_number_reflns         12366
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0414
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0529P)^2^+3.2018P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1026
_refine_ls_wR_factor_ref         0.1080
_reflns_number_gt                10812
_reflns_number_total             12366
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt02115d2.cif
_cod_data_source_block           '[Pd(4)](PF6)2'
_cod_depositor_comments
'Adding full bibliography for 7035701--7035705.cif.'
_cod_original_cell_volume        2114.67(15)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7035704