A very large Rh?Rh bond shortening on excitation of the [Rh2(1,8-diisocyano-p-menthane)4]2+ ion by time-resolved synchrotron X-ray diffraction
Coppens, Philip; Gerlits, Oksana; Vorontsov, Ivan I.; Kovalevsky, Andrey Yu.; Chen, Yu-Sheng; Graber, Tim; Gembicky, Milan; Novozhilova, Irina V.; Chemical Communications  (2004) 2144–2145; doi:10.1039/b409463h

data_7111424
_publ_section_title
;
 A very large Rh?Rh bond shortening on excitation of the
 [Rh2(1,8-diisocyano-p-menthane)4]2+ ion by time-resolved synchrotron
 X-ray diffraction
;
_journal_issue                   19
_journal_name_full               'Chemical Communications'
_journal_page_first              2144
_journal_page_last               2145
_journal_paper_doi               10.1039/b409463h
_journal_year                    2004
_chemical_formula_moiety         'C48 H72 N8 Rh2 2+, 2(F6 P 1-), C2 H3 N'
_chemical_formula_sum            'C50 H75 F12 N9 P2 Rh2'
_chemical_formula_weight         1297.95
_chemical_name_common            '[Rh2(dimen)4](PF6)2xCH3CN'
_chemical_name_systematic
;
dirhodium(I) tetrakis-1,8-diisocyano-p-menthane hexafluorophosphate
acetonitrile solvate
;
_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                61.9167(7)
_cell_angle_beta                 84.9358(8)
_cell_angle_gamma                75.0680(11)
_cell_formula_units_Z            1
_cell_length_a                   9.4407(6)
_cell_length_b                   13.4608(6)
_cell_length_c                   13.6781(8)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    16(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      4
_cell_volume                     1480.66(14)
_computing_cell_refinement       'SAINTPlus (Bruker, 1998a)'
_computing_data_collection       'SMART (Bruker, 1998b)'
_computing_data_reduction        'SAINTPlus (Bruker, 1998a)'
_computing_molecular_graphics    'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_computing_publication_material  'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_computing_structure_refinement  'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_computing_structure_solution    'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_diffrn_ambient_temperature      16(2)
_diffrn_measured_fraction_theta_full 0.847
_diffrn_measured_fraction_theta_max 0.847
_diffrn_measurement_device_type  'Bruker SMART 6000 CCD area detector'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_monochromator  diamond
_diffrn_radiation_source         undulator
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.49594
_diffrn_reflns_av_R_equivalents  0.0196
_diffrn_reflns_av_sigmaI/netI    0.0312
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17062
_diffrn_reflns_theta_full        21.97
_diffrn_reflns_theta_max         21.97
_diffrn_reflns_theta_min         1.18
_exptl_absorpt_coefficient_mu    0.369
_exptl_absorpt_correction_T_max  0.9890
_exptl_absorpt_correction_T_min  0.9640
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS(Sheldrick, 1998a)'
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             666
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.363
_refine_diff_density_min         -1.084
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         9024
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0357
_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^)+(0.0565P)^2^+0.8449P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.0936
_reflns_number_gt                8153
_reflns_number_total             9024
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b409463hsup1.cif
_cod_data_source_block           dimen1300
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'multi-scans' was replaced
with the value 'multi-scan' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
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_cod_database_code               7111424