Photochemical Reactions of Fluorinated Pyridines at Half-Sandwich Rhodium Complexes: Competing Pathways of Reaction.
Procacci, Barbara; Blagg, Robin J.; Perutz, Robin N.; Rendón, Nuria; Whitwood, Adrian C.; Organometallics 33 (2014) 45–52; doi:10.1021/om400552r

data_4082609
_publ_section_title
;
 Photochemical Reactions of Fluorinated Pyridines at Half-Sandwich Rhodium
 Complexes: Competing Pathways of Reaction.
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              45
_journal_page_last               52
_journal_paper_doi               10.1021/om400552r
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C13 H15 F4 N P Rh'
_chemical_formula_sum            'C13 H15 F4 N P Rh'
_chemical_formula_weight         395.14
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-05-23
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 106.8831(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.54836(14)
_cell_length_b                   8.63903(11)
_cell_length_c                   16.43266(19)
_cell_measurement_reflns_used    7655
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      32.1428
_cell_measurement_theta_min      3.0975
_cell_volume                     1432.93(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      110.00(10)
_diffrn_detector_area_resol_mean 16.1450
_diffrn_measured_fraction_theta_full 0.9980
_diffrn_measured_fraction_theta_max 0.9821
_diffrn_measurement_details
;
  1 omega -100.00  -62.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.1672 -178.0000   60.0000 38

  2 omega  -21.00   88.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.5735    0.0000   60.0000 109

  3 omega  -17.00   76.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.5735   19.0000  150.0000 93

  4 omega  -94.00  -49.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.1672  -57.0000 -120.0000 45

  5 omega  -46.00   71.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.5735  -19.0000  -60.0000 117
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0317509000
_diffrn_orient_matrix_UB_12      0.0371529000
_diffrn_orient_matrix_UB_13      0.0391376000
_diffrn_orient_matrix_UB_21      -0.0526944000
_diffrn_orient_matrix_UB_22      -0.0225944000
_diffrn_orient_matrix_UB_23      0.0161601000
_diffrn_orient_matrix_UB_31      0.0339500000
_diffrn_orient_matrix_UB_32      -0.0696314000
_diffrn_orient_matrix_UB_33      0.0155617000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            13834
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         32.22
_diffrn_reflns_theta_min         3.10
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.336
_exptl_absorpt_correction_T_max  0.906
_exptl_absorpt_correction_T_min  0.762
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'dark yellow'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.832
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             784
_exptl_crystal_recrystallization_method 'slow evaporation of hexane/benzene'
_exptl_crystal_size_max          0.3359
_exptl_crystal_size_mid          0.2592
_exptl_crystal_size_min          0.1033
_refine_diff_density_max         1.579
_refine_diff_density_min         -0.727
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         4625
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0255
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0222P)^2^+0.9744P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0560
_refine_ls_wR_factor_ref         0.0601
_reflns_number_gt                4007
_reflns_number_total             4625
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400552r_si_002.cif
_cod_data_source_block           rnp1310
_cod_database_code               4082609
_chemical_oxdiff_formula         'C13 H15 F4 N1 P1 Rh1'
_chemical_oxdiff_usercomment     'Barbara's CpRh9PMe3)(H)(C5F4N)'
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_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.a Ternary CH refined with riding coordinates:
 C13(H13), C12(H12), C11(H11), C10(H10), C9(H9)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C7(H7A,H7B,H7C), C6(H6A,H6B,H6C)
;