A new structural type of dinuclear rhodium(II) compounds: synthesis by serendipity and design; catalytic behaviour in carbene transfer reactions †
Estevan, Francisco; García-Bernabé, Abel; García-Granda, Santiago; Lahuerta, Pascual; Moreno, Eduardo; Pérez-Prieto, Julia; Sanaú, Mercedes; Ubeda, M. Angeles; Journal of the Chemical Society, Dalton Transactions  (1999) 3493–; doi:10.1039/a903811f

data_7027541
_publ_section_title
;
 A new structural type of dinuclear rhodium(II) compounds: synthesis by
 serendipity and design; catalytic behaviour in carbene transfer
 reactions&#x200A;&#x2020;
;
_journal_issue                   19
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3493
_journal_paper_doi               10.1039/a903811f
_journal_year                    1999
_chemical_formula_moiety         'C42 H40 Cl2 O6 P2 Rh2, (3/2CH2Cl2)'
_chemical_formula_sum            'C43.5 H43 Cl5 O6 P2 Rh2'
_chemical_formula_weight         1106.79
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 94.8900(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.9125(10)
_cell_length_b                   13.0427(8)
_cell_length_c                   19.6074(12)
_cell_measurement_temperature    293(2)
_cell_volume                     4564.2(5)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens Smart CCD'
_diffrn_measurement_method       '\w scans\'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0553
_diffrn_reflns_av_sigmaI/netI    0.0549
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16640
_diffrn_reflns_theta_max         23.33
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    1.132
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2228
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.235
_refine_diff_density_min         -3.341
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.090
_refine_ls_goodness_of_fit_obs   1.136
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         6475
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_restrained_S_obs      1.136
_refine_ls_R_factor_all          0.0952
_refine_ls_R_factor_obs          0.0768
_refine_ls_shift/esd_max         0.230
_refine_ls_shift/esd_mean        0.015
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0843P)^2^+54.8599P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2031
_refine_ls_wR_factor_obs         0.1895
_reflns_number_observed          5256
_reflns_number_total             6475
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            903811fsup1.cif
_cod_data_source_block           COMPOUND4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_crystal_density_meas' value 'no' 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0843P)^2^+54.8599P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0843P)^2^+54.8599P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C43.50 H43 Cl5 O6 P2 Rh2'
_cod_database_code               7027541