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_7010240
_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            'C19 H24 Br2 N4 O Pd'
_chemical_formula_weight         590.66
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90.00000
_cell_angle_beta                 106.661(3)
_cell_angle_gamma                90.00000
_cell_formula_units_Z            4
_cell_length_a                   11.207(3)
_cell_length_b                   13.300(3)
_cell_length_c                   15.434(3)
_cell_measurement_reflns_used    5847
_cell_measurement_temperature    293
_cell_measurement_theta_max      26.4
_cell_measurement_theta_min      2
_cell_volume                     2203.9(9)
_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      293
_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  .044
_diffrn_reflns_av_sigmaI/netI    .097
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            25643
_diffrn_reflns_theta_max         29.08
_diffrn_reflns_theta_min         1.9
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.48
_exptl_absorpt_correction_T_max  .802
_exptl_absorpt_correction_T_min  .407
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS; Sheldrick, 1996
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.78
_exptl_crystal_description       block
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          .40
_exptl_crystal_size_mid          .30
_exptl_crystal_size_min          .20
_refine_diff_density_max         .936
_refine_diff_density_min         -1.085
_refine_ls_extinction_coef       94(192)
_refine_ls_extinction_expression 'Eq22 p292 "Cryst. Comp." Munksgaard 1970'
_refine_ls_extinction_method     Zachariasen
_refine_ls_goodness_of_fit_all   1.228
_refine_ls_goodness_of_fit_ref   1.402
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3828
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .07
_refine_ls_R_factor_gt           .039
_refine_ls_shift/su_max          .04
_refine_ls_shift/su_mean         .002
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .051
_refine_ls_wR_factor_ref         .047
_reflns_d_resolution_high        .731
_reflns_d_resolution_low         10.714
_reflns_limit_h_max              15
_reflns_limit_h_min              0
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              -21
_reflns_number_gt                3828
_reflns_number_total             5589
_reflns_threshold_expression     'F    > 4.00 sig(F   )'
_cod_data_source_file            b007293l.txt
_cod_data_source_block           ccw167
_cod_original_sg_symbol_Hall     -p_2ybc
_cod_original_sg_symbol_H-M      p_1_21/c_1
_cod_original_formula_sum        'C19 H24 Br2 N4 O1 Pd1'
_cod_database_code               7010240