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_4031978
_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
'C45 H57 N2 P Rh, 0.5(C7 H8), B F4, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C49 H62 B Cl F4 N2 P Rh'
_chemical_formula_weight         935.14
_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   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_vv12
_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 17:38:51 CET UTC+01:00  encif 1.38'
_cell_angle_alpha                107.751(13)
_cell_angle_beta                 96.045(9)
_cell_angle_gamma                96.260(13)
_cell_formula_units_Z            4
_cell_length_a                   10.903(4)
_cell_length_b                   17.768(7)
_cell_length_c                   24.913(9)
_cell_measurement_reflns_used    7874
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.22
_cell_measurement_theta_min      2.31
_cell_volume                     4520(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 0.930
_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  0.0376
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            117410
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.930
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.485
_diffrn_reflns_theta_min         0.868
_diffrn_source                   'sealed X-Ray tube (Mo)'
_diffrn_source_type              'fine focus tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.525
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6974
_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    1.374
_exptl_crystal_description       block
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         2.207
_refine_diff_density_min         -1.111
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1096
_refine_ls_number_reflns         30412
_refine_ls_number_restraints     100
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0427
_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^)+(0.0465P)^2^+6.7591P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1030
_refine_ls_wR_factor_ref         0.1155
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22684
_reflns_number_total             30412
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1860-5397-12-83-S2.cif
_cod_data_source_block           ga_vv12
_cod_depositor_comments
'Adding full bibliography for 4031975--4031986.cif.'
_cod_database_code               4031978
_audit_block_refno               2347
_audit_block_usercomment         VV107
_shelx_estimated_absorpt_t_max   0.925
_shelx_estimated_absorpt_t_min   0.893
_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
 C99A-Cl1 \\sim C99A-Cl2 \\sim C99B-Cl1 \\sim C99B-Cl2
 with sigma of 0.02
 B1-F1 \\sim B1-F2 \\sim B1-F3 \\sim B1-F4 \\sim B51-F51 \\sim B51-F52 \\sim
B51-F53 \\sim B51-F54
 with sigma of 0.02
 F1-F2 \\sim F1-F3 \\sim F1-F4 \\sim F2-F3 \\sim F2-F4 \\sim F3-F4 \\sim
F51-F52 \\sim F51-F53 \\sim F51-F54 ~
 F52-F53 \\sim F52-F54 \\sim F53-F54
 with sigma of 0.02
3. Others
 Sof(C99B)=Sof(H99C)=Sof(H99D)=1-FVAR(1)
 Sof(C99A)=Sof(H99A)=Sof(H99B)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C8(H8), C11(H11), C20(H20), C23(H23), C38(H38), C39(H39), C42(H42), C43(H43),
 C58(H58), C61(H61), C70(H70), C73(H73), C88(H88), C89(H89), C92(H92), C93(H93)
4.b Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B), C41(H41A,H41B), C44(H44A,H44B), C45(H45A,H45B), C90(H90A,
 H90B), C91(H91A,H91B), C94(H94A,H94B), C95(H95A,H95B), C99A(H99A,H99B),
 C99B(H99C,H99D)
4.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C16(H16), C17(H17), C18(H18), C27(H27), C28(H28),
 C29(H29), C30(H30), C31(H31), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37),
  C54(H54), C55(H55), C56(H56), C66(H66), C67(H67), C68(H68), C77(H77),
 C78(H78), C79(H79), C80(H80), C81(H81), C83(H83), C84(H84), C85(H85), C86(H86),
  C87(H87), C102(H102), C103(H103), C104(H104), C105(H105), C106(H106)
4.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C25(H25A,
 H25B,H25C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C62(H62A,H62B,H62C),
 C63(H63A,H63B,H63C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C74(H74A,H74B,
 H74C), C75(H75A,H75B,H75C), C107(H10D,H10E,H10F)
;
_shelx_res_checksum              30569
_olex2_submission_special_instructions 'No special instructions were received'