Crystal structure of dichlorotriethylphosphine{12- (3,4-dimethoxyphenyl)- 4,5-dimethoxy-11,14-diaza-tricyclo[7.4.1.0^2,7^]tetradeca-2(7),3,5- trien-10-one}palladium(II) methanol solvate, PdCl~2~[P(C~2~H~5~)~3~] (C~22~H~26~N~2~O~5~) · CH~3~OH
B. Miller; M. Rüth; K. Polborn; W. Steglich; W. Beck; Zeitschrift für Kristallographie - New Crystal Structures 220 (2005) 145–146; doi:

data_8101723
_publ_section_title
;
Crystal structure of dichlorotriethylphosphine{12- (3,4-dimethoxyphenyl)-
4,5-dimethoxy-11,14-diaza-tricyclo[7.4.1.0^2,7^]tetradeca-2(7),3,5-
trien-10-one}palladium(II) methanol solvate, PdCl~2~[P(C~2~H~5~)~3~]
(C~22~H~26~N~2~O~5~) &#x00B7; CH~3~OH
;
_journal_issue                   2
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              145
_journal_page_last               146
_journal_volume                  220
_journal_year                    2005
_chemical_formula_sum            'C29 H45 Cl2 N2 O6 P Pd'
_chemical_formula_weight         725.94
_chemical_name_systematic
; 
dichloro-triethylphosphine-12-(3,4-dimethoxyphenyl)-4,5-dimethoxy-
11,13-diaza-tricyclo[7.3.1.0^2,7^]trideca-2(7),3,5-trien-10-one-
palladium(II)
;
_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
_cell_angle_alpha                83.99(2)
_cell_angle_beta                 76.596(13)
_cell_angle_gamma                86.558(12)
_cell_formula_units_Z            2
_cell_length_a                   8.4763(7)
_cell_length_b                   13.135(2)
_cell_length_c                   15.418(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      9
_cell_volume                     1659.5(4)
_computing_cell_refinement       'CAD4 (Nonius, 1977)'
_computing_data_collection       'CAD4 (Nonius, 1977)'
_computing_data_reduction        'process MOLEN (Fair, 1990)'
_computing_molecular_graphics    'ZORTEP (Zsolnai, 1994)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       omega-2theta
_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  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0258
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5576
_diffrn_reflns_theta_max         23.97
_diffrn_reflns_theta_min         2.47
_diffrn_standards_decay_%        -2.2
_diffrn_standards_interval_time  7200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.810
_exptl_absorpt_correction_T_max  0.9991
_exptl_absorpt_correction_T_min  0.8807
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            pale_yellow
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_description       bloc
_exptl_crystal_F_000             752
_exptl_crystal_size_max          .27
_exptl_crystal_size_mid          .23
_exptl_crystal_size_min          .17
_refine_diff_density_max         0.338
_refine_diff_density_min         -0.644
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.044
_refine_ls_goodness_of_fit_obs   1.054
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         5180
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_restrained_S_obs      1.054
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_obs          0.0336
_refine_ls_shift/esd_max         -0.023
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0392P)^2^+1.8586P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0865
_refine_ls_wR_factor_obs         0.0803
_reflns_number_observed          4431
_reflns_number_total             5180
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            1267-1462.cff
_cod_data_source_block           miller4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0392P)^2^+1.8586P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0392P)^2^+1.8586P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1659.5(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               8101723