#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:37:32 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179799 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/95/7009501.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7009501
loop_
_publ_author_name
'Burrows, Andrew D.'
'Mahon, Mary F.'
'Palmer, Mark T.'
_publ_section_title
;
 Ether functionalised aminophosphines: synthesis and co-ordination
 chemistry of palladium(II) and platinum(II) complexes †
;
_journal_issue                   10
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1669
_journal_paper_doi               10.1039/b001436m
_journal_year                    2000
_chemical_formula_sum            'C30 H36 Cl2 N2 O2 P2 Pd'
_chemical_formula_weight         695.85
_chemical_name_systematic
;

  ?

;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 100.641(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.456(2)
_cell_length_b                   7.5530(10)
_cell_length_c                   19.935(2)
_cell_measurement_temperature    150(2)
_cell_volume                     1547.3(4)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      396(2)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0904
_diffrn_reflns_av_sigmaI/netI    0.0729
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            6352
_diffrn_reflns_theta_max         24.95
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    0.906
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.830
_refine_diff_density_min         -0.907
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.146
_refine_ls_goodness_of_fit_obs   1.250
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         2395
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.146
_refine_ls_restrained_S_obs      1.250
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_obs          0.0383
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0541P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1098
_refine_ls_wR_factor_obs         0.1084
_reflns_number_observed          1992
_reflns_number_total             2395
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b001436m.txt
_cod_data_source_block           Complex1
_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:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0541P)^2^+0.0000P] 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^)+(0.0541P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7009501
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Pd1 Pd 0.0000 0.0000 0.5000 0.0108(2) Uani 1 d S .
P1 P -0.17096(9) 0.16750(13) 0.44220(5) 0.0134(3) Uani 1 d . .
Cl1 Cl 0.10103(10) -0.00004(11) 0.40704(5) 0.0193(3) Uani 1 d . .
N1 N -0.2263(3) 0.3065(4) 0.4935(2) 0.0185(8) Uani 1 d D .
H1 H -0.2281(43) 0.2645(53) 0.5365(15) 0.030(13) Uiso 1 d D .
O1 O -0.3172(3) 0.5094(3) 0.5910(2) 0.0269(8) Uani 1 d . .
C1 C -0.2977(4) 0.0155(4) 0.4031(2) 0.0168(9) Uani 1 d . .
C2 C -0.2689(4) -0.1132(5) 0.3576(2) 0.0228(10) Uani 1 d . .
H2 H -0.1860(4) -0.1190(5) 0.3471(2) 0.027 Uiso 1 calc R .
C3 C -0.3642(4) -0.2324(5) 0.3284(2) 0.0291(11) Uani 1 d . .
H3 H -0.3456(4) -0.3167(5) 0.2976(2) 0.035 Uiso 1 calc R .
C4 C -0.4859(4) -0.2258(6) 0.3448(3) 0.0338(12) Uani 1 d . .
H4 H -0.5493(4) -0.3058(6) 0.3249(3) 0.041 Uiso 1 calc R .
C5 C -0.5150(4) -0.1015(6) 0.3905(3) 0.0338(12) Uani 1 d . .
H5 H -0.5974(4) -0.0981(6) 0.4018(3) 0.041 Uiso 1 calc R .
C6 C -0.4203(4) 0.0179(5) 0.4194(2) 0.0251(11) Uani 1 d . .
H6 H -0.4397(4) 0.1013(5) 0.4503(2) 0.030 Uiso 1 calc R .
C7 C -0.1403(4) 0.3081(4) 0.3731(2) 0.0134(9) Uani 1 d . .
C8 C -0.0511(4) 0.4460(5) 0.3896(2) 0.0208(10) Uani 1 d . .
H8 H -0.0116(4) 0.4641(5) 0.4349(2) 0.025 Uiso 1 calc R .
C9 C -0.0213(4) 0.5557(6) 0.3393(2) 0.0237(10) Uani 1 d . .
H9 H 0.0366(4) 0.6490(6) 0.3509(2) 0.028 Uiso 1 calc R .
C10 C -0.0772(4) 0.5274(5) 0.2719(2) 0.0237(10) Uani 1 d . .
H10 H -0.0550(4) 0.5992(5) 0.2379(2) 0.028 Uiso 1 calc R .
C11 C -0.1657(4) 0.3928(5) 0.2552(2) 0.0241(10) Uani 1 d . .
H11 H -0.2044(4) 0.3747(5) 0.2099(2) 0.029 Uiso 1 calc R .
C12 C -0.1978(4) 0.2837(5) 0.3055(2) 0.0202(10) Uani 1 d . .
H12 H -0.2584(4) 0.1936(5) 0.2938(2) 0.024 Uiso 1 calc R .
C13 C -0.3212(4) 0.4489(5) 0.4746(2) 0.0243(10) Uani 1 d . .
H13A H -0.4087(4) 0.4016(5) 0.4695(2) 0.029 Uiso 1 calc R .
H13B H -0.3107(4) 0.5000(5) 0.4313(2) 0.029 Uiso 1 calc R .
C14 C -0.3011(4) 0.5902(5) 0.5294(2) 0.0235(10) Uani 1 d . .
H14A H -0.2145(4) 0.6403(5) 0.5340(2) 0.028 Uiso 1 calc R .
H14B H -0.3642(4) 0.6846(5) 0.5175(2) 0.028 Uiso 1 calc R .
C15 C -0.2983(5) 0.6297(6) 0.6467(3) 0.0368(12) Uani 1 d . .
H15A H -0.3027(30) 0.5668(9) 0.6881(3) 0.055 Uiso 1 calc R .
H15B H -0.3650(18) 0.7187(24) 0.6391(8) 0.055 Uiso 1 calc R .
H15C H -0.2146(13) 0.6849(31) 0.6505(10) 0.055 Uiso 1 calc R .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 Pd1 Cl1 180.0 3_556 . ?
Cl1 Pd1 P1 88.49(4) 3_556 . ?
Cl1 Pd1 P1 91.51(4) . . ?
Cl1 Pd1 P1 91.51(4) 3_556 3_556 ?
Cl1 Pd1 P1 88.49(4) . 3_556 ?
P1 Pd1 P1 180.0 . 3_556 ?
N1 P1 C7 103.3(2) . . ?
N1 P1 C1 110.9(2) . . ?
C7 P1 C1 105.1(2) . . ?
N1 P1 Pd1 111.59(13) . . ?
C7 P1 Pd1 117.98(12) . . ?
C1 P1 Pd1 107.65(12) . . ?
C13 N1 P1 127.6(3) . . ?
C14 O1 C15 112.5(3) . . ?
C6 C1 C2 118.8(4) . . ?
C6 C1 P1 121.8(3) . . ?
C2 C1 P1 119.3(3) . . ?
C3 C2 C1 119.9(4) . . ?
C4 C3 C2 120.1(4) . . ?
C3 C4 C5 120.6(4) . . ?
C4 C5 C6 119.3(4) . . ?
C1 C6 C5 121.2(4) . . ?
C12 C7 C8 118.8(4) . . ?
C12 C7 P1 123.8(3) . . ?
C8 C7 P1 117.4(3) . . ?
C9 C8 C7 120.4(4) . . ?
C10 C9 C8 120.2(4) . . ?
C11 C10 C9 119.7(4) . . ?
C10 C11 C12 120.4(4) . . ?
C7 C12 C11 120.4(4) . . ?
N1 C13 C14 109.6(3) . . ?
O1 C14 C13 107.5(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 Cl1 2.2963(10) 3_556 ?
Pd1 Cl1 2.2963(10) . ?
Pd1 P1 2.3158(10) . ?
Pd1 P1 2.3158(10) 3_556 ?
P1 N1 1.643(3) . ?
P1 C7 1.815(4) . ?
P1 C1 1.817(4) . ?
N1 C13 1.464(5) . ?
O1 C14 1.410(5) . ?
O1 C15 1.420(5) . ?
C1 C6 1.379(6) . ?
C1 C2 1.400(6) . ?
C2 C3 1.389(6) . ?
C3 C4 1.371(6) . ?
C4 C5 1.381(7) . ?
C5 C6 1.383(6) . ?
C7 C12 1.381(6) . ?
C7 C8 1.397(5) . ?
C8 C9 1.380(6) . ?
C9 C10 1.379(6) . ?
C10 C11 1.375(6) . ?
C11 C12 1.386(6) . ?
C13 C14 1.513(6) . ?
