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_4031977
_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         'C39 H45 N2 P Rh, B F4, C H2 Cl2'
_chemical_formula_sum            'C40 H47 B Cl2 F4 N2 P Rh'
_chemical_formula_weight         847.38
_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_vv4
_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 17:04:23 CET UTC+01:00  encif 1.38'
_cell_angle_alpha                89.234(11)
_cell_angle_beta                 89.261(14)
_cell_angle_gamma                89.370(9)
_cell_formula_units_Z            4
_cell_length_a                   12.435(5)
_cell_length_b                   15.735(7)
_cell_length_c                   19.553(8)
_cell_measurement_reflns_used    8066
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.06
_cell_measurement_theta_min      2.34
_cell_volume                     3825(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 0.984
_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  0.0484
_diffrn_reflns_av_unetI/netI     0.0493
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            98486
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.506
_diffrn_reflns_theta_min         1.638
_diffrn_source                   'sealed X-Ray tube (Mo)'
_diffrn_source_type              'fine focus tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.679
_exptl_absorpt_correction_T_max  0.9039
_exptl_absorpt_correction_T_min  0.8467
_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    1.471
_exptl_crystal_description       block
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.130
_refine_diff_density_max         1.590
_refine_diff_density_min         -1.039
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     983
_refine_ls_number_reflns         25065
_refine_ls_number_restraints     168
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0399
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0410P)^2^+3.8552P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0891
_refine_ls_wR_factor_ref         0.0990
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19118
_reflns_number_total             25065
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1860-5397-12-83-S2.cif
_cod_data_source_block           ga_vv4
_cod_depositor_comments
'Adding full bibliography for 4031975--4031986.cif.'
_cod_database_code               4031977
_audit_block_refno               2307
_audit_block_usercomment         tr1533
_shelx_estimated_absorpt_t_max   0.917
_shelx_estimated_absorpt_t_min   0.876
_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
 B2-F21 \\sim B2-F22 \\sim B2-F23 \\sim B2-F24 \\sim B2-F32 \\sim B2-F33 \\sim
B2-F34
 with sigma of 0.02
 F21-F22 \\sim F21-F23 \\sim F21-F24 \\sim F22-F23 \\sim F22-F24 \\sim F23-F24
\\sim F21-F32 \\sim F21-F33
 \\sim F21-F34 \\sim F32-F33 \\sim F32-F34 \\sim F33-F34
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 B2, F21, F22, F23, F24, F32, F33, F34
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Same fragment restrains
{Cl11, Cl12, C91} sigma for 1-2: 0.02, 1-3: 0.04
as
{Cl21, Cl22, C92}
5. Others
 Sof(F33)=Sof(F34)=Sof(F32)=1-FVAR(1)
 Sof(F22)=Sof(F23)=Sof(F24)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C34(H34A,H34B), C35(H35A,H35B), C38(H38A,H38B), C39(H39A,H39B), C84(H84A,
 H84B), C85(H85A,H85B), C89(H89A,H89B), C90(H90A,H90B), C91(H91A,H91B),
 C92(H92A,H92B)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C6(H6), C13(H13), C15(H15), C21(H21), C22(H22), C23(H23),
 C24(H24), C25(H25), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C51(H51),
  C54(H54), C56(H56), C63(H63), C65(H65), C71(H71), C72(H72), C73(H73),
 C74(H74), C75(H75), C77(H77), C78(H78), C79(H79), C80(H80), C81(H81)
6.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C17(H17A,H17B,H17C),
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C58(H58A,H58B,H58C), C59(H59A,H59B,
 H59C), C60(H60A,H60B,H60C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C69(H69A,
 H69B,H69C)
;
_shelx_res_checksum              83809
_olex2_submission_special_instructions 'No special instructions were received'