Double cyclometallation of bis[3-(3-bromophenyl)pyrazol-1-yl]methane in the bis[acetylacetonatopalladium(II)] complex
Olga Juanes; Juan-Carlos Rodriguez-Ubis; César J. Pastor; Acta Crystallographica Section E 57 (2001) m595–m596; doi:10.1107/S1600536801019419

data_2200808
_publ_section_title
;
 Double cyclometallation of bis[3-(3-bromophenyl)pyrazol-1-yl]methane
 in the bis[acetylacetonatopalladium(II)] complex
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m595
_journal_page_last               m596
_journal_paper_doi               10.1107/S1600536801019419
_journal_volume                  57
_journal_year                    2001
_chemical_formula_iupac
'[Pd2 (C5 H7 O2)2 (C19 H12 Br2 N4)], 0.5C2 H3 N'
_chemical_formula_moiety         'C29 H26 Br2 N4 O4 Pd2, 0.5C2 H3 N'
_chemical_formula_sum            'C30 H27.5 Br2 N4.5 O4 Pd2'
_chemical_formula_weight         887.66
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 120.536(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   35.262(3)
_cell_length_b                   8.3791(5)
_cell_length_c                   24.9461(17)
_cell_measurement_reflns_used    55
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      45.0
_cell_measurement_theta_min      5.5
_cell_volume                     6348.4(9)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Bruker, 2000)'
_computing_data_reduction        'SHELXTL (Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      297(2)
_diffrn_measured_fraction_theta_full .988
_diffrn_measured_fraction_theta_max .988
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  .040
_diffrn_reflns_av_sigmaI/netI    .031
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            5165
_diffrn_reflns_theta_full        56.8
_diffrn_reflns_theta_max         56.8
_diffrn_reflns_theta_min         2.9
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    12.44
_exptl_absorpt_correction_T_max  .929
_exptl_absorpt_correction_T_min  .377
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details   '(XPREP; Bruker, 2000)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.858
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             3464
_exptl_crystal_size_max          .18
_exptl_crystal_size_mid          .15
_exptl_crystal_size_min          .12
_refine_diff_density_max         2.45
_refine_diff_density_min         -1.10
_refine_ls_extinction_coef       .000049(9)
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.12
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         4209
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.12
_refine_ls_R_factor_all          .060
_refine_ls_R_factor_gt           .055
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0563P)^2^+138.5779P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .143
_reflns_number_gt                3848
_reflns_number_total             4209
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ya6071.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        6348.4(8)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2200808
_cod_database_fobs_code          2200808