A modular approach to neutral P,N-ligands: synthesis and coordination chemistry.
Vasilenko, Vladislav; Roth, Torsten; Blasius, Clemens K.; Intorp, Sebastian N.; Wadepohl, Hubert; Gade, Lutz H.; Beilstein journal of organic chemistry 12 (2016) 846–853; doi:10.3762/bjoc.12.83

data_4031976
_publ_section_title
;
 A modular approach to neutral P,N-ligands: synthesis and coordination
 chemistry.
;
_journal_name_full               'Beilstein journal of organic chemistry'
_journal_page_first              846
_journal_page_last               853
_journal_paper_doi               10.3762/bjoc.12.83
_journal_volume                  12
_journal_year                    2016
_chemical_formula_moiety
'C62 H66 Cl2 N4 P2 Pd2, 2(B F4), C H2 Cl2, 0.5(C7 H8)'
_chemical_formula_sum            'C66.5 H72 B2 Cl4 F8 N4 P2 Pd2'
_chemical_formula_weight         1517.44
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_vv2
_audit_creation_date             2016-01-25
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record             '25.01.2016 16:52:38 CET UTC+01:00  encif 1.38'
_cell_angle_alpha                82.724(8)
_cell_angle_beta                 80.839(13)
_cell_angle_gamma                87.563(12)
_cell_formula_units_Z            2
_cell_length_a                   11.291(6)
_cell_length_b                   13.841(7)
_cell_length_c                   21.603(10)
_cell_measurement_reflns_used    8016
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.96
_cell_measurement_theta_min      2.33
_cell_volume                     3305(3)
_computing_cell_refinement
;
SAINT (see _computing_data_reduction). Includes estimated systematic errors
 of the unit cell constants from Monte Carlo simulations.
;
_computing_data_collection       'SMART-5.631 (Bruker AXS, 2003)'
_computing_data_reduction
'SAINT V8.34A (Bruker AXS, 1997-2013),SADABS-2014_4 (Sheldrick and Bruker AXS, 1997-2014)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material
'encif (Wadepohl, 2009-15); encifer 1.5 (CCDC, 2014)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_environment      'perfluoro polyether oil / N~2~'
_diffrn_ambient_temperature      100(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.19
_diffrn_detector_type            CCD-PXL-KAF2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker AXS Smart 1000'
_diffrn_measurement_method       '\f- and \w-scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.918
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            65911
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.918
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.435
_diffrn_reflns_theta_min         1.864
_diffrn_source                   'sealed X-Ray tube (Mo)'
_diffrn_source_type              'fine focus tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.821
_exptl_absorpt_correction_T_max  0.8828
_exptl_absorpt_correction_T_min  0.8021
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements (Blessing 1995)
SADABS (see _computing_data_reduction)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_description       needle
_exptl_crystal_F_000             1542
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.110
_refine_diff_density_max         2.234
_refine_diff_density_min         -1.702
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     876
_refine_ls_number_reflns         21848
_refine_ls_number_restraints     222
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0465
_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/[\s^2^(Fo^2^)+(0.0451P)^2^+8.9965P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1188
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17078
_reflns_number_total             21848
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1860-5397-12-83-S2.cif
_cod_data_source_block           ga_vv2
_cod_depositor_comments
'Adding full bibliography for 4031975--4031986.cif.'
_cod_original_formula_sum        'C66.50 H72 B2 Cl4 F8 N4 P2 Pd2'
_cod_database_code               4031976
_audit_block_refno               2295
_audit_block_usercomment         VV43_3
_shelx_estimated_absorpt_t_max   0.915
_shelx_estimated_absorpt_t_min   0.827
_shelxl_version_number           2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 B1-F11 \\sim B1-F12 \\sim B1-F13 \\sim B1-F14
 with sigma of 0.02
 F11-F12 \\sim F11-F13 \\sim F11-F14 \\sim F12-F13 \\sim F12-F14 \\sim F13-F14
 with sigma of 0.02
 B2A-F21A \\sim B2A-F22A \\sim B2A-F23A \\sim B2A-F24A \\sim B2B-F21B \\sim
B2B-F22B \\sim B2B-F23B ~
 B2B-F24B
 with sigma of 0.001
 F21A-F22A \\sim F21A-F23A \\sim F21A-F24A \\sim F22A-F23A \\sim F22A-F24A
\\sim F23A-F24A \\sim F21B-
 F22B \\sim F21B-F23B \\sim F21B-F24B \\sim F22B-F23B \\sim F22B-F24B \\sim
F23B-F24B
 with sigma of 0.001
 C92-C97 \\sim C96-C97
 with sigma of 0.01
3. Restrained atomic chiral volume
 C91
 fixed at 0 with sigma of 0.1
4. Rigid body (RIGU) restrains
 F21A, F22A, F23A, F24A, B2A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F21B, F22B, F23B, F24B, B2B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C91, C92, C93, C94, C95, C96, C97
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F21B)=Sof(F22B)=Sof(F23B)=Sof(F24B)=Sof(B2B)=1-FVAR(1)
 Sof(F21A)=Sof(F22A)=Sof(F23A)=Sof(F24A)=Sof(B2A)=FVAR(1)
 Fixed Sof: C91(0.5) C92(0.5) H92(0.5) C93(0.5) H93(0.5) C94(0.5) H94(0.5)
 C95(0.5) H95(0.5) C96(0.5) H96(0.5) C97(0.5) H97A(0.5) H97B(0.5) H97C(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C81(H81A,H81B)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C6(H6), C13(H13), C15(H15), C20(H20), C21(H21), C22(H22),
 C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31),
  C34(H34), C36(H36), C43(H43), C45(H45), C51(H51), C52(H52), C53(H53),
 C54(H54), C55(H55), C57(H57), C58(H58), C59(H59), C60(H60), C61(H61), C92(H92),
  C93(H93), C94(H94), C95(H95), C96(H96)
6.c Fitted hexagon refined as free rotating group:
 C91(C92,C93,C94,C95,C96)
6.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C16(H16A,H16B,H16C),
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C38(H38A,H38B,H38C), C39(H39A,H39B,
 H39C), C40(H40A,H40B,H40C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C49(H49A,
 H49B,H49C), C97(H97A,H97B,H97C)
;
_shelx_res_checksum              21170
_olex2_submission_special_instructions 'No special instructions were received'