<i>cis</i>-Dichloridobis{[(<i>S</i>)-<i>N</i>-(3,5-dioxa-4-phosphacyclohepta[2,1-<i>a</i>;3,4-<i>a</i>']dinaphthalen-4-yl]dibenz[<i>b</i>,<i>f</i>]azepin-κ<i>P</i>}palladium(II) deuterochloroform disolvate
Alexander Briceño; Romano Dorta; Acta Crystallographica Section E 63 (2007) m1718–m1719; doi:10.1107/S1600536807023173

data_2213796
_publ_section_title
;<i>cis</i>-Dichloridobis{[(<i>S</i>)-<i>N</i>-(3,5-dioxa-4-phosphacyclohepta[2,1-<i>a</i>;3,4-<i>a</i>']dinaphthalen-4-yl]dibenz[<i>b</i>,<i>f</i>]azepin-\k<i>P</i>}palladium(II)
 deuterochloroform disolvate
;
_journal_coeditor_code           HB2403
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1718
_journal_page_last               m1719
_journal_paper_doi               10.1107/S1600536807023173
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Pd Cl2 (C34 H22 N O2 P)2].2CD Cl3'
_chemical_formula_moiety         'C68 H44 Cl2 N2 O4 P2 Pd, 2(C D Cl3)'
_chemical_formula_sum            'C70 H44 Cl8 D2 N2 O4 P2 Pd'
_chemical_formula_weight         1431.03
_chemical_name_systematic
;
Dichlorido-
<i>cis</i>-bis[{(<i>S</i>)-(3,5-dioxa-4-phosphacyclohepta[2,1-a;3,4
-a']dinaphthalen-4-yl)dibenz[b,f]azepin}-\\k<i>P</i>]palladium(II)
deuterochloroform disolvate
;
_space_group_IT_number           76
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4w'
_symmetry_space_group_name_H-M   'P 41'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.866(2)
_cell_length_b                   19.866(2)
_cell_length_c                   17.497(2)
_cell_measurement_reflns_used    2378
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.60
_cell_measurement_theta_min      1.98
_cell_volume                     6905.3(13)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2000)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC Inc., 2004)'
_computing_molecular_graphics
;
SHELXLTL-NT and DIAMOND
(Brandenburg, 1998)
;
_computing_publication_material
;
SHELXLTL-NT and PLATON (Spek, 2003)
;
_computing_structure_refinement  SHELXLTL-NT
_computing_structure_solution    'SHELXLTL-NT (Bruker, 1998)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 14.6306
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.889
_diffrn_measurement_device
;
Mercury (2x2 bin mode)
;
_diffrn_measurement_device_type  'Rigaku AFC7S Mercury'
_diffrn_measurement_method       '\w '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0628
_diffrn_reflns_av_sigmaI/netI    0.0659
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            79958
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.03
_diffrn_reflns_theta_min         1.45
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.672
_exptl_absorpt_correction_T_max  0.891
_exptl_absorpt_correction_T_min  0.802
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson (1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2896
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.058
_refine_diff_density_min         -0.715
_refine_ls_abs_structure_details 'Flack (1983), with 5079 Friedel pairs'
_refine_ls_abs_structure_Flack   0.02(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     886
_refine_ls_number_reflns         14408
_refine_ls_number_restraints     593
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1280
_refine_ls_R_factor_gt           0.0738
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1446P)^2^+3.0373P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1922
_refine_ls_wR_factor_ref         0.2480
_reflns_number_gt                9124
_reflns_number_total             14408
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb2403.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed
to 'multi-scan' 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 'Tetragonal' changed to 'tetragonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' 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        6905.2(13)
_cod_database_code               2213796
_cod_database_fobs_code          2213796