Palladium carbene complexes derived from imidazolium-linked ortho-cyclophanes
Baker, Murray V.; Skelton, Brian W.; White, Allan H.; Williams, Charlotte C.; Journal of the Chemical Society, Dalton Transactions  (2001) 111–; doi:10.1039/b007293l

data_7010238
_publ_section_title
;
 Palladium carbene complexes derived from imidazolium-linked
 ortho-cyclophanes
;
_journal_issue                   2
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              111
_journal_paper_doi               10.1039/b007293l
_journal_year                    2001
_chemical_formula_sum            'C22.5 H22 I2 N4 O0.5 Pd'
_chemical_formula_weight         716.68
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90.00000
_cell_angle_beta                 95.946(2)
_cell_angle_gamma                90.00000
_cell_formula_units_Z            4
_cell_length_a                   10.3800(10)
_cell_length_b                   8.9810(10)
_cell_length_c                   25.693(3)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    153
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     2382.3(4)
_computing_cell_refinement       'Siemens SAINT (Siemens, 1995)'
_computing_data_collection       'Siemens SMART (Siemens, 1995)'
_computing_data_reduction        'xtal ADDREF SORTRF'
_computing_molecular_graphics    xtal
_computing_publication_material  'xtal BONDLA CIFIO'
_computing_structure_refinement  'xtal CRYLSQ'
_computing_structure_solution    xtal
_diffrn_ambient_temperature      153
_diffrn_measurement_device_type
;
Bruker SMART CCD diffractometer
;
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_detector       'CCD area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .042
_diffrn_reflns_av_sigmaI/netI    .01
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            26807
_diffrn_reflns_theta_max         29.01
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    3.39
_exptl_absorpt_correction_T_max  .802
_exptl_absorpt_correction_T_min  .502
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS; Sheldrick, 1996
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.998
_exptl_crystal_description       plate
_exptl_crystal_F_000             1364
_exptl_crystal_size_max          .4
_exptl_crystal_size_mid          .38
_exptl_crystal_size_min          .08
_refine_diff_density_max         1.496
_refine_diff_density_min         -1.056
_refine_ls_extinction_coef       1001(142)
_refine_ls_extinction_expression 'Eq22 p292 "Cryst. Comp." Munksgaard 1970'
_refine_ls_extinction_method     Zachariasen
_refine_ls_goodness_of_fit_all   1.248
_refine_ls_goodness_of_fit_ref   1.259
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     278
_refine_ls_number_reflns         5744
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .032
_refine_ls_R_factor_gt           .031
_refine_ls_shift/su_max          .043
_refine_ls_shift/su_mean         .002
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .045
_refine_ls_wR_factor_ref         .044
_reflns_d_resolution_high        .733
_reflns_d_resolution_low         9.917
_reflns_Friedel_coverage         0
_reflns_limit_h_max              14
_reflns_limit_h_min              0
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              33
_reflns_limit_l_min              -34
_reflns_number_gt                5744
_reflns_number_total             5935
_reflns_threshold_expression     'F    > 4.00 sig(F   )'
_cod_data_source_file            b007293l.txt
_cod_data_source_block           cwi
_cod_original_sg_symbol_Hall     -p_2yn
_cod_original_sg_symbol_H-M      P_1_21/n_1
_cod_original_formula_sum        'C22.5 H22 I2 N4 O.5 Pd1'
_cod_database_code               7010238