A dimer of bis(N-heterocyclic carbene)rhodium(I) centres spanned by a dibenzo-18-crown-6 bridge from synchrotron radiation
Shrestha, Sumi; Bhadbhade, Mohan; Gimbert-Suriñach, Carolina; Colbran, Stephen B.; Acta Crystallographica Section E 69 (2013) m47–m48; doi:10.1107/S160053681204901X

data_2237234
_publ_section_title
;
 A dimer of bis(N-heterocyclic carbene)rhodium(I) centres spanned by a
 dibenzo-18-crown-6 bridge from synchrotron radiation
;
_journal_coeditor_code           TK5170
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m47
_journal_page_last               m48
_journal_paper_doi               10.1107/S160053681204901X
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac
'[Rh2 (C8 H12)2 (C40 H42 N8 O6)] (P F6)2, 1.5C2 H3 N, 2H2 O'
_chemical_formula_moiety
'C56 H66 N8 O6 Rh2 2+, 2(F6 P -), 1.5(C2 H3 N), 2(H2 O)'
_chemical_formula_sum            'C59 H74.5 F12 N9.5 O8 P2 Rh2'
_chemical_formula_weight         1540.55
_chemical_name_common
;
[(L){Rh(COD)}~2~][PF~6~]~2~ (L = bis{4,5-bis(1-methylene-3-
methylimidazolidene)}benzo-18-crown-6; COD = 1,5-cyclooctadiene)
;
_chemical_name_systematic
;
(\m-3,3',3'',3'''-{[2,5,8,15,18,21-
Hexaoxatricyclo[20.4.0.0^9,14^]hexacosa-1(22),9,11,13,23,25-hexaene-
11,12,24,25-tetrayl]tetrakis(methylene)}tetrakis(1-methyl-1<i>H</i>-imidazol-
2-yl))bis[(\h^4^-cycloocta-1,4-diene)rhodium(I)] bis(hexafluoridophosphate)
acetonitrile sesquisolvate dihydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                104.69(3)
_cell_angle_beta                 90.20(3)
_cell_angle_gamma                109.58(3)
_cell_formula_units_Z            2
_cell_length_a                   10.510(2)
_cell_length_b                   15.630(3)
_cell_length_c                   23.280(5)
_cell_measurement_reflns_used    9980
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      2.5
_cell_volume                     3468.9(15)
_computing_cell_refinement       '<i>XDS</i> (Kabsch, 1993)'
_computing_data_collection
'<i>BLU-ICE</i> (McPhillips <i>et al.</i>, 2002)'
_computing_data_reduction        '<i>XDS</i> (Kabsch, 1993)'
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008) and <i>OLEX2</i> (Dolomanov <i>et al.</i>,
2009)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.938
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  '3-BM1 Australian Synchrotron'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  Si<111>
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0305
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            43942
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.82
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.611
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             1574
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.153
_refine_diff_density_min         -1.402
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.333
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     964
_refine_ls_number_reflns         11473
_refine_ls_number_restraints     270
_refine_ls_restrained_S_all      1.334
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0509
_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^)+(0.1000P)^2^+0.5989P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1588
_refine_ls_wR_factor_ref         0.1642
_reflns_number_gt                9939
_reflns_number_total             11473
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tk5170.cif
_cod_data_source_block           I
_cod_original_cell_volume        3468.9(12)
_cod_database_code               2237234
_cod_database_fobs_code          2237234