#------------------------------------------------------------------------------
#$Date: 2019-11-17 11:29:13 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229594 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/52/7045222.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_7045222
loop_
_publ_author_name
'Cullinane, Carleen'
'Deacon, Glen B.'
'Drago, Penny R.'
'Erven, Anja P.'
'Junk, Peter C.'
'Luu, Jenny'
'Meyer, Gerd'
'Schmitz, Simon'
'Ott, Ingo'
'Schur, Julia'
'Webster, Lorraine K.'
'Klein, Axel'
_publ_section_title
;
 Synthesis and antiproliferative activity of a series of new platinum and
 palladium diphosphane complexes.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1918
_journal_page_last               1932
_journal_paper_doi               10.1039/c7dt04615d
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C30 H32 F8 N2 Pd'
_chemical_formula_sum            'C30 H32 F8 N2 Pd'
_chemical_formula_weight         678.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-12-06 deposited with the CCDC.
2018-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.44(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.907(5)
_cell_length_b                   8.4520(17)
_cell_length_c                   13.096(3)
_cell_measurement_reflns_used    18028
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.52
_cell_measurement_theta_min      2.96
_cell_volume                     2638.3(10)
_computing_cell_refinement       'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7085
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18028
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.438
_diffrn_reflns_theta_min         2.952
_diffrn_standards_decay_%        'not measured'
_diffrn_standards_interval_count 'not measured'
_diffrn_standards_interval_time  'not measured'
_diffrn_standards_number         'not measured'
_exptl_absorpt_coefficient_mu    0.785
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.480
_refine_diff_density_min         -0.817
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         2690
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0277
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0304P)²+7.8526P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0713
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2617
_reflns_number_total             2690
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt04615d2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7045222--7045225.cif.'
_cod_original_cell_volume        2638.3(9)
_cod_database_code               7045222
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Pd1 Pd 0.5000 0.55723(2) 0.7500 0.01411(9) Uani 1 2 d S T P
F1 F 0.43257(6) 0.44914(15) 0.55252(10) 0.0229(3) Uani 1 1 d . . .
F3 F 0.36696(6) 0.07936(15) 0.85969(10) 0.0228(3) Uani 1 1 d . . .
F4 F 0.44631(6) 0.29161(16) 0.90075(9) 0.0230(3) Uani 1 1 d . . .
F2 F 0.35053(5) 0.24515(17) 0.51233(9) 0.0237(3) Uani 1 1 d . . .
N1 N 0.30768(9) 0.0584(3) 0.66284(16) 0.0321(5) Uani 1 1 d . . .
C1 C 0.56278(9) 0.7602(3) 0.79846(17) 0.0203(4) Uani 1 1 d . . .
H1 H 0.5984 0.7230 0.8358 0.024 Uiso 1 1 calc R U .
C11 C 0.44265(8) 0.3834(2) 0.72917(16) 0.0158(4) Uani 1 1 d . . .
C2 C 0.56099(9) 0.7400(3) 0.69469(17) 0.0203(4) Uani 1 1 d . . .
H8 H 0.5960 0.6935 0.6701 0.024 Uiso 1 1 calc R U .
C3 C 0.52552(9) 0.8286(3) 0.61345(17) 0.0223(5) Uani 1 1 d . . .
H7A H 0.5192 0.7593 0.5527 0.027 Uiso 1 1 calc R U .
H7B H 0.5469 0.9220 0.5927 0.027 Uiso 1 1 calc R U .
C16 C 0.42325(9) 0.2840(2) 0.80264(15) 0.0161(4) Uani 1 1 d . . .
C15 C 0.38140(9) 0.1734(2) 0.78197(15) 0.0170(4) Uani 1 1 d . . .
C8 C 0.53200(10) 0.8853(3) 0.85507(17) 0.0228(5) Uani 1 1 d . . .
H2A H 0.5264 0.9798 0.8108 0.027 Uiso 1 1 calc R U .
H2B H 0.5555 0.9170 0.9173 0.027 Uiso 1 1 calc R U .
C14 C 0.35357(9) 0.1557(2) 0.68499(16) 0.0170(4) Uani 1 1 d . . .
C13 C 0.37443(9) 0.2524(3) 0.60977(15) 0.0172(4) Uani 1 1 d . . .
C12 C 0.41695(9) 0.3593(2) 0.63175(15) 0.0164(4) Uani 1 1 d . . .
C33 C 0.20018(10) -0.0637(3) 0.58983(18) 0.0226(5) Uani 1 1 d . . .
H17A H 0.1631 -0.0424 0.5535 0.027 Uiso 1 1 calc R U .
H17B H 0.2013 -0.1764 0.6103 0.027 Uiso 1 1 calc R U .
C35 C 0.30371(10) -0.0479(3) 0.57502(17) 0.0227(5) Uani 1 1 d . . .
H19A H 0.3095 -0.1585 0.5985 0.027 Uiso 1 1 calc R U .
H19B H 0.3332 -0.0216 0.5288 0.027 Uiso 1 1 calc R U .
C31 C 0.26642(10) 0.0269(3) 0.73688(17) 0.0235(5) Uani 1 1 d . . .
H15A H 0.2712 0.1039 0.7939 0.028 Uiso 1 1 calc R U .
H15B H 0.2723 -0.0807 0.7656 0.028 Uiso 1 1 calc R U .
C34 C 0.24627(10) -0.0315(3) 0.51783(17) 0.0221(5) Uani 1 1 d . . .
H18A H 0.2429 -0.1073 0.4601 0.027 Uiso 1 1 calc R U .
H18B H 0.2419 0.0768 0.4895 0.027 Uiso 1 1 calc R U .
C32 C 0.20766(10) 0.0401(3) 0.68506(18) 0.0233(5) Uani 1 1 d . . .
H16A H 0.2001 0.1517 0.6656 0.028 Uiso 1 1 calc R U .
H16B H 0.1801 0.0081 0.7339 0.028 Uiso 1 1 calc R U .
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9850 1.0430 '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
C11 Pd1 C11 86.29(12) . 2_656
C11 Pd1 C2 153.72(8) . .
C11 Pd1 C2 95.28(8) 2_656 .
C11 Pd1 C2 95.28(8) . 2_656
C11 Pd1 C2 153.72(8) 2_656 2_656
C2 Pd1 C2 94.70(11) . 2_656
C11 Pd1 C1 171.72(8) . .
C11 Pd1 C1 94.74(8) 2_656 .
C2 Pd1 C1 34.43(8) . .
C2 Pd1 C1 80.17(8) 2_656 .
C11 Pd1 C1 94.74(8) . 2_656
C11 Pd1 C1 171.72(8) 2_656 2_656
C2 Pd1 C1 80.17(8) . 2_656
C2 Pd1 C1 34.43(8) 2_656 2_656
C1 Pd1 C1 85.43(11) . 2_656
C14 N1 C35 122.27(19) . .
C14 N1 C31 122.32(19) . .
C35 N1 C31 113.94(18) . .
C2 C1 C8 126.5(2) . .
C2 C1 Pd1 70.63(12) . .
C8 C1 Pd1 108.64(14) . .
C2 C1 H1 114.1 . .
C8 C1 H1 114.1 . .
Pd1 C1 H1 114.1 . .
C16 C11 C12 113.70(19) . .
C16 C11 Pd1 127.58(15) . .
C12 C11 Pd1 118.68(15) . .
C1 C2 C3 127.8(2) . .
C1 C2 Pd1 74.94(13) . .
C3 C2 Pd1 102.83(14) . .
C1 C2 H8 114.0 . .
C3 C2 H8 114.0 . .
Pd1 C2 H8 114.0 . .
C2 C3 C8 115.49(18) . 2_656
C2 C3 H7A 108.4 . .
C8 C3 H7A 108.4 2_656 .
C2 C3 H7B 108.4 . .
C8 C3 H7B 108.4 2_656 .
H7A C3 H7B 107.5 . .
F4 C16 C15 116.85(18) . .
F4 C16 C11 119.68(18) . .
C15 C16 C11 123.46(19) . .
F3 C15 C16 118.17(18) . .
F3 C15 C14 119.27(19) . .
C16 C15 C14 122.56(19) . .
C1 C8 C3 113.00(18) . 2_656
C1 C8 H2A 109.0 . .
C3 C8 H2A 109.0 2_656 .
C1 C8 H2B 109.0 . .
C3 C8 H2B 109.0 2_656 .
H2A C8 H2B 107.8 . .
N1 C14 C15 124.7(2) . .
N1 C14 C13 121.3(2) . .
C15 C14 C13 114.00(18) . .
F2 C13 C12 118.49(18) . .
F2 C13 C14 119.17(18) . .
C12 C13 C14 122.30(19) . .
F1 C12 C13 116.71(18) . .
F1 C12 C11 119.41(18) . .
C13 C12 C11 123.84(19) . .
C32 C33 C34 110.96(19) . .
C32 C33 H17A 109.4 . .
C34 C33 H17A 109.4 . .
C32 C33 H17B 109.4 . .
C34 C33 H17B 109.4 . .
H17A C33 H17B 108.0 . .
N1 C35 C34 109.5(2) . .
N1 C35 H19A 109.8 . .
C34 C35 H19A 109.8 . .
N1 C35 H19B 109.8 . .
C34 C35 H19B 109.8 . .
H19A C35 H19B 108.2 . .
N1 C31 C32 109.8(2) . .
N1 C31 H15A 109.7 . .
C32 C31 H15A 109.7 . .
N1 C31 H15B 109.7 . .
C32 C31 H15B 109.7 . .
H15A C31 H15B 108.2 . .
C35 C34 C33 110.29(19) . .
C35 C34 H18A 109.6 . .
C33 C34 H18A 109.6 . .
C35 C34 H18B 109.6 . .
C33 C34 H18B 109.6 . .
H18A C34 H18B 108.1 . .
C31 C32 C33 111.72(19) . .
C31 C32 H16A 109.3 . .
C33 C32 H16A 109.3 . .
C31 C32 H16B 109.3 . .
C33 C32 H16B 109.3 . .
H16A C32 H16B 107.9 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 C11 2.014(2) .
Pd1 C11 2.014(2) 2_656
Pd1 C2 2.281(2) .
Pd1 C2 2.281(2) 2_656
Pd1 C1 2.335(2) .
Pd1 C1 2.335(2) 2_656
F1 C12 1.361(2) .
F3 C15 1.357(2) .
F4 C16 1.360(2) .
F2 C13 1.359(2) .
N1 C14 1.384(3) .
N1 C35 1.457(3) .
N1 C31 1.460(3) .
C1 C2 1.367(3) .
C1 C8 1.515(3) .
C1 H1 1.0000 .
C11 C16 1.384(3) .
C11 C12 1.388(3) .
C2 C3 1.507(3) .
C2 H8 1.0000 .
C3 C8 1.542(3) 2_656
C3 H7A 0.9900 .
C3 H7B 0.9900 .
C16 C15 1.381(3) .
C15 C14 1.395(3) .
C8 C3 1.542(3) 2_656
C8 H2A 0.9900 .
C8 H2B 0.9900 .
C14 C13 1.401(3) .
C13 C12 1.374(3) .
C33 C32 1.524(3) .
C33 C34 1.529(3) .
C33 H17A 0.9900 .
C33 H17B 0.9900 .
C35 C34 1.519(3) .
C35 H19A 0.9900 .
C35 H19B 0.9900 .
C31 C32 1.516(3) .
C31 H15A 0.9900 .
C31 H15B 0.9900 .
C34 H18A 0.9900 .
C34 H18B 0.9900 .
C32 H16A 0.9900 .
C32 H16B 0.9900 .
