Double cyclometallation of bis[3-(3-methoxyphenyl)pyrazol-1-yl]methane in a bis[(acetylacetonato)palladium(II)] complex
Olga Juanes; Juan-Carlos Rodriguez-Ubis; César J. Pastor; Acta Crystallographica Section E 57 (2001) m576–m577; doi:10.1107/S1600536801018712

data_2200805
_publ_section_title
;
 Double cyclometallation of bis[3-(3-methoxyphenyl)pyrazol-1-yl]methane
 in a bis[(acetylacetonato)palladium(II)] complex
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m576
_journal_page_last               m577
_journal_paper_doi               10.1107/S1600536801018712
_journal_volume                  57
_journal_year                    2001
_chemical_formula_iupac          '[Pd2 (C5 H7 O2)2 (C21 H18 N4 O2)]'
_chemical_formula_moiety         'C31 H32 N4 O6 Pd2'
_chemical_formula_sum            'C31 H32 N4 O6 Pd2'
_chemical_formula_weight         769.41
_chemical_name_systematic
;
 ?
;
_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'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 115.156(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.3726(7)
_cell_length_b                   14.6998(11)
_cell_length_c                   15.9304(9)
_cell_measurement_reflns_used    68
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      47.5
_cell_measurement_theta_min      6.8
_cell_volume                     3046.5(3)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1996)'
_computing_data_reduction        'SHELXTL (Sheldrick, 1997b)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full .985
_diffrn_measured_fraction_theta_max .985
_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  .027
_diffrn_reflns_av_sigmaI/netI    .025
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4996
_diffrn_reflns_theta_full        56.7
_diffrn_reflns_theta_max         56.7
_diffrn_reflns_theta_min         3.5
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    9.94
_exptl_absorpt_correction_T_max  .779
_exptl_absorpt_correction_T_min  .341
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details   '(XPREP; Bruker, 2000)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular_cut
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          .35
_exptl_crystal_size_mid          .25
_exptl_crystal_size_min          .15
_refine_diff_density_max         1.26
_refine_diff_density_min         -.65
_refine_ls_extinction_coef       .00038(4)
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.07
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         4011
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.07
_refine_ls_R_factor_all          .035
_refine_ls_R_factor_gt           .033
_refine_ls_shift/su_max          .006
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0519P)^2^+4.3327P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .088
_reflns_number_gt                3777
_reflns_number_total             4011
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ya6067.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_sg_symbol_H-M      'P 21/n'
_cod_database_code               2200805
_cod_database_fobs_code          2200805