A convenient method for the generation of {Rh(PNP)}<sup>+</sup> and {Rh(PONOP)}<sup>+</sup> fragments: reversible formation of vinylidene derivatives.
Gyton, Matthew R.; Hood, Thomas M.; Chaplin, Adrian B.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 2877–2880; doi:10.1039/c8dt05049j

data_7048902
_publ_section_title
;
 A convenient method for the generation of {Rh(PNP)}<sup>+</sup> and
 {Rh(PONOP)}<sup>+</sup> fragments: reversible formation of vinylidene
 derivatives.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2877
_journal_page_last               2880
_journal_paper_doi               10.1039/c8dt05049j
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C27 H49 N O2 P2 Rh, C32 H12 B F24'
_chemical_formula_sum            'C59 H61 B F24 N O2 P2 Rh'
_chemical_formula_weight         1447.74
_chemical_melting_point          ?
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-12-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-12-20 deposited with the CCDC.
2019-01-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.4584(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.77010(19)
_cell_length_b                   18.6612(2)
_cell_length_c                   27.1605(4)
_cell_measurement_reflns_used    23195
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.3200
_cell_measurement_theta_min      2.5440
_cell_volume                     6443.14(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2833
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -58.00   69.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       23.1653  -19.0000 -180.0000 127

  2 omega  -53.00   50.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       23.1653  -38.0000  -60.0000 103

  3 omega -103.00    9.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      -24.2590  -77.0000  -30.0000 112

  4 omega -114.00  -57.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      -24.2590 -178.0000    0.0000 57

  5 omega   -3.00   99.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       23.1653   38.0000  -90.0000 102

  6 omega  -98.00  -16.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      -24.2590  -57.0000   90.0000 82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction: Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0335019000
_diffrn_orient_matrix_UB_12      0.0020497000
_diffrn_orient_matrix_UB_13      -0.0223289000
_diffrn_orient_matrix_UB_21      -0.0446314000
_diffrn_orient_matrix_UB_22      -0.0011732000
_diffrn_orient_matrix_UB_23      0.0136615000
_diffrn_orient_matrix_UB_31      0.0004350000
_diffrn_orient_matrix_UB_32      0.0379375000
_diffrn_orient_matrix_UB_33      0.0016318000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0530
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            83031
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        27.102
_diffrn_reflns_theta_max         27.102
_diffrn_reflns_theta_min         3.014
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.425
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86185
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2936
_exptl_crystal_recrystallization_method
'Crystals grown from 1,2-C6H4F2-hexane at 293 K'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.721
_refine_diff_density_min         -0.811
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1027
_refine_ls_number_reflns         14184
_refine_ls_number_restraints     1008
_refine_ls_restrained_S_all      1.196
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0435
_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^)+(0.0526P)^2^+6.0494P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1034
_refine_ls_wR_factor_ref         0.1125
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11127
_reflns_number_total             14184
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt05049j3.cif
_cod_data_source_block           0187abc15
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7048901--7048908.cif.
;
_cod_original_cell_volume        6443.13(16)
_cod_database_code               7048902
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C207-F1 \\sim C207-F2 \\sim C207-F3 \\sim C207-F1A \\sim C207-F2A \\sim
C207-F3A
 with sigma of 0.01
 F1-F2 \\sim F2-F3 \\sim F3-F1 \\sim F1A-F2A \\sim F2A-F3A \\sim F3A-F1A
 with sigma of 0.01
 C203-F1 \\sim C203-F2 \\sim C203-F3 \\sim C203-F1A \\sim C203-F2A \\sim
C203-F3A
 with sigma of 0.01
 C208-F4 \\sim C208-F5 \\sim C208-F6 \\sim C208-F4A \\sim C208-F5A \\sim
C208-F6A
 with sigma of 0.01
 F4-F5 \\sim F5-F6 \\sim F6-F4 \\sim F4A-F5A \\sim F5A-F6A \\sim F6A-F4A
 with sigma of 0.01
 C205-F4 \\sim C205-F5 \\sim C205-F6 \\sim C205-F4A \\sim C205-F5A \\sim
C205-F6A
 with sigma of 0.01
 C215-F7 \\sim C215-F8 \\sim C215-F9 \\sim C215-F7A \\sim C215-F8A \\sim
C215-F9A
 with sigma of 0.01
 F7-F8 \\sim F8-F9 \\sim F9-F7 \\sim F7A-F8A \\sim F8A-F9A \\sim F9A-F7A
 with sigma of 0.01
 C211-F7 \\sim C211-F8 \\sim C211-F9 \\sim C211-F7A \\sim C211-F8A \\sim
C211-F9A
 with sigma of 0.01
 C216-F10 \\sim C216-F11 \\sim C216-F12 \\sim C216-F10A \\sim C216-F11A \\sim
C216-F12A
 with sigma of 0.01
 F10-F11 \\sim F11-F12 \\sim F12-F10 \\sim F10A-F11A \\sim F11A-F12A \\sim
F12A-F10A
 with sigma of 0.01
 C213-F10 \\sim C213-F11 \\sim C213-F12 \\sim C213-F10A \\sim C213-F11A \\sim
C213-F12A
 with sigma of 0.01
 C231-F19 \\sim C231-F20 \\sim C231-F21 \\sim C231-F19A \\sim C231-F20A \\sim
C231-F21A
 with sigma of 0.01
 F19-F20 \\sim F20-F21 \\sim F21-F19 \\sim F19A-F20A \\sim F20A-F21A \\sim
F21A-F19A
 with sigma of 0.01
 C227-F19 \\sim C227-F20 \\sim C227-F21 \\sim C227-F19A \\sim C227-F20A \\sim
C227-F21A
 with sigma of 0.01
 C232-F22 \\sim C232-F23 \\sim C232-F24 \\sim C232-F22A \\sim C232-F23A \\sim
C232-F24A
 with sigma of 0.01
 F22-F23 \\sim F23-F24 \\sim F24-F22 \\sim F22A-F23A \\sim F23A-F24A \\sim
F24A-F22A
 with sigma of 0.01
 C229-F22 \\sim C229-F23 \\sim C229-F24 \\sim C229-F22A \\sim C229-F23A \\sim
C229-F24A
 with sigma of 0.01
 Rh1-C4A \\sim Rh1-C4
 with sigma of 0.005
 C5A-C4A \\sim C5-C4
 with sigma of 0.005
 C6A-C5A \\sim C6-C5
 with sigma of 0.015
 C7-C6 \\sim C9A-C6A \\sim C8-C6 \\sim C8A-C6A \\sim C9-C6 \\sim C7A-C6A
 with sigma of 0.015
 C7-C5 \\sim C9A-C5A \\sim C8-C5 \\sim C8A-C5A \\sim C9-C5 \\sim C7A-C5A
 with sigma of 0.015
 C7-C8 \\sim C8-C9 \\sim C9-C7 \\sim C7A-C8A \\sim C8A-C9A \\sim C9A-C7A
 with sigma of 0.015
3. Uiso/Uaniso restraints and constraints
C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9 \\sim C5A \\sim C6A \\sim C7A
\\sim C8A \\sim C9A \\sim F1 \\sim F1A \\sim F2 \\sim F2A \\sim F3 \\sim F3A
\\sim F4 \\sim F4A \\sim F5 \\sim F5A \\sim F6 \\sim F6A \\sim F7 \\sim F7A
\\sim F8 \\sim F8A \\sim F9 \\sim F9A \\sim F10 \\sim F10A \\sim F11 \\sim F11A
\\sim F12 \\sim F12A \\sim F13 \\sim F14 \\sim F15 \\sim F16 \\sim F17 \\sim
F18 \\sim F19 \\sim F19A \\sim F20 \\sim F20A \\sim F21 \\sim F21A \\sim F22
\\sim F22A \\sim F23 \\sim F23A \\sim F24 \\sim F24A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim
Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C5A) \\sim Ueq, Uanis(C6A)
\\sim Ueq, Uanis(C7A) \\sim Ueq, Uanis(C8A) \\sim Ueq, Uanis(C9A) \\sim Ueq,
Uanis(F1) \\sim Ueq, Uanis(F1A) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F2A)
\\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F3A) \\sim Ueq, Uanis(F4) \\sim Ueq,
Uanis(F4A) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F5A) \\sim Ueq, Uanis(F6)
\\sim Ueq, Uanis(F6A) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F7A) \\sim Ueq,
Uanis(F8) \\sim Ueq, Uanis(F8A) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F9A)
\\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F10A) \\sim Ueq, Uanis(F11) \\sim Ueq,
Uanis(F11A) \\sim Ueq, Uanis(F12) \\sim Ueq, Uanis(F12A) \\sim Ueq, Uanis(F13)
\\sim Ueq, Uanis(F14) \\sim Ueq, Uanis(F15) \\sim Ueq, Uanis(F16) \\sim Ueq,
Uanis(F17) \\sim Ueq, Uanis(F18) \\sim Ueq, Uanis(F19) \\sim Ueq, Uanis(F19A)
\\sim Ueq, Uanis(F20) \\sim Ueq, Uanis(F20A) \\sim Ueq, Uanis(F21) \\sim Ueq,
Uanis(F21A) \\sim Ueq, Uanis(F22) \\sim Ueq, Uanis(F22A) \\sim Ueq, Uanis(F23)
\\sim Ueq, Uanis(F23A) \\sim Ueq, Uanis(F24) \\sim Ueq, Uanis(F24A) \\sim Ueq:
with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C6A) = Uanis(C6)
Uanis(C9A) = Uanis(C8)
Uanis(C8A) = Uanis(C9)
Uanis(C4) = Uanis(C4A)
4. Others
 Sof(F22A)=Sof(F23A)=Sof(F24A)=1-FVAR(1)
 Sof(F22)=Sof(F23)=Sof(F24)=FVAR(1)
 Sof(F19A)=Sof(F20A)=Sof(F21A)=1-FVAR(2)
 Sof(F19)=Sof(F20)=Sof(F21)=FVAR(2)
 Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(3)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(3)
 Sof(F10A)=Sof(F11A)=Sof(F12A)=1-FVAR(4)
 Sof(F10)=Sof(F11)=Sof(F12)=FVAR(4)
 Sof(F7A)=Sof(F8A)=Sof(F9A)=1-FVAR(5)
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(5)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=1-FVAR(6)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(6)
 Fixed Sof: C4(0.5) C4A(0.5) C5(0.5) H5(0.5) C5A(0.5) H5A(0.5) C6(0.5)
 C6A(0.5) C7(0.5) H7A(0.5) H7B(0.5) H7C(0.5) C7A(0.5) H7AA(0.5) H7AB(0.5)
 H7AC(0.5) C8(0.5) H8A(0.5) H8B(0.5) H8C(0.5) C8A(0.5) H8AA(0.5) H8AB(0.5)
 H8AC(0.5) C9(0.5) H9A(0.5) H9B(0.5) H9C(0.5) C9A(0.5) H9AA(0.5) H9AB(0.5)
 H9AC(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C5A(H5A), C22(H22), C23(H23), C24(H24), C202(H202), C204(H204),
 C206(H206), C210(H210), C212(H212), C214(H214), C218(H218), C220(H220),
 C222(H222), C226(H226), C228(H228), C230(H230)
5.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C7A(H7AA,H7AB,H7AC), C8(H8A,H8B,H8C), C8A(H8AA,H8AB,H8AC),
 C9(H9A,H9B,H9C), C9A(H9AA,H9AB,H9AC), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C),
  C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,
 H35C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,
 H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C)
;
_shelx_res_checksum              63845
_olex2_submission_special_instructions 'No special instructions were received'