Bis{[3-(diphenylphosphino)propyl]trimethylphosphonium-<i>P</i>}[(2,3,5,6-η)-norbornadiene]rhodium(I) Tris(tetrafluoroborate)
Roszak, A. W.; Renaud, E.; Baird, M. C.; Acta Crystallographica Section C 52 (1996) 1359–1362; doi:10.1107/S0108270195017069

data_2004977
_publ_section_title
;Bis{[3-(diphenylphosphino)propyl]trimethylphosphonium-<i>P</i>}[(2,3,5,6-\h)-norbornadiene]rhodium(I)
 Tris(tetrafluoroborate)
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1359
_journal_page_last               1362
_journal_paper_doi               10.1107/S0108270195017069
_journal_volume                  52
_journal_year                    1996
_chemical_formula_iupac          '[Rh (C18 H25 P2)2 (C7 H8)] (B1 F4)3'
_chemical_formula_moiety         'C43 H58 P4 Rh, 3(B F4)'
_chemical_formula_structural     '[Rh(C~7~H~8~)(C~18~H~25~P~2~)~2~](BF~4~)~3~'
_chemical_formula_sum            'C43 H58 B3 F12 P4 Rh'
_chemical_formula_weight         1062.11
_chemical_name_common            '[NBDRh(II-phophos)~2~](BF~4~)~3~'
_chemical_name_systematic
;
Bis{2-(diphenylphosphinoethyl)trimethylphosphonium}(norbornadiene)rhodium(I)
Fluoroborate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                116.340(10)
_cell_angle_beta                 124.840(10)
_cell_angle_gamma                75.360(10)
_cell_formula_units_Z            2
_cell_length_a                   14.021(2)
_cell_length_b                   15.613(2)
_cell_length_c                   15.430(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.6
_cell_measurement_theta_min      13.2
_cell_volume                     2484.5(7)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'Xtal3.0 (Hall & Stewart, 1990)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_sigmaI/netI    0.0549
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11273
_diffrn_reflns_theta_max         26.97
_diffrn_reflns_theta_min         1.46
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.547
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.809
_refine_diff_density_min         -0.374
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.112
_refine_ls_goodness_of_fit_obs   1.155
_refine_ls_hydrogen_treatment
'H atoms riding (SHELXL93 defaults, C---H 0.93--0.98\%A)'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     724
_refine_ls_number_reflns         10824
_refine_ls_number_restraints     360
_refine_ls_restrained_S_all      1.139
_refine_ls_restrained_S_obs      1.199
_refine_ls_R_factor_all          0.0962
_refine_ls_R_factor_obs          0.0495
_refine_ls_shift/esd_max         0.012
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
calc w = 1/[\s^2^(F~o~^2^) + (0.0814P)^2^]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1591
_refine_ls_wR_factor_obs         0.1228
_reflns_number_observed          6255
_reflns_number_total             10824
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            fg1107.cif
_cod_data_source_block           mb1
_cod_depositor_comments
;
The following automatic conversions were performed:

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

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        2484.5(6)
_cod_database_code               2004977