Mixed anhydride complexes of rhodium(i) and ruthenium(ii) - their synthesis and ligand rearrangements.
Coetzee, Jacorien; Eastham, Graham R.; Slawin, Alexandra M. Z.; Cole-Hamilton, David J; Dalton transactions (Cambridge, England : 2003) 43 (2014) 3479–3491; doi:10.1039/c3dt52552j

data_7029125
_publ_section_title
;
 Mixed anhydride complexes of rhodium(i) and ruthenium(ii) - their
 synthesis and ligand rearrangements.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3479
_journal_page_last               3491
_journal_paper_doi               10.1039/c3dt52552j
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C67 H75 Cl O4 P3 Rh'
_chemical_formula_sum            'C67 H75 Cl O4 P3 Rh'
_chemical_formula_weight         1175.54
_chemical_name_common
;
Chloro(propanoyl-(3,3',5,5'-tetra-tert-butyl-1,1'-biphenyl-
2,2'-diyl)phosphite)bis(triphenylphosphine)rhodium(I)
;
_chemical_name_systematic
; 
Chloro(propanoyl-(3,3',5,5'-tetra-tert-butyl-1,1'-biphenyl-
2,2'-diyl)phosphite)bis(triphenylphosphine)rhodium(I) 
;
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.147(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.139(4)
_cell_length_b                   11.654(2)
_cell_length_c                   23.570(5)
_cell_measurement_reflns_used    21685
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      29.1
_cell_measurement_theta_min      1.5
_cell_volume                     6004.3(19)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2004)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2004)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2004)'
_computing_molecular_graphics
'X-seed (Barbour 2001; Atwood and Barbour 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.877
_diffrn_measurement_device_type  'Rigaku Saturn724 (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1740
_diffrn_reflns_av_sigmaI/netI    0.1621
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            51481
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.08
_diffrn_reflns_theta_min         1.07
_exptl_absorpt_coefficient_mu    0.456
_exptl_absorpt_correction_T_max  0.9909
_exptl_absorpt_correction_T_min  0.8753
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2464
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.436
_refine_diff_density_min         -0.915
_refine_diff_density_rms         0.198
_refine_ls_extinction_coef       0.0033(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.274
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     687
_refine_ls_number_reflns         14097
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.274
_refine_ls_R_factor_all          0.1818
_refine_ls_R_factor_gt           0.1326
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0994P)^2^+21.5669P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2890
_refine_ls_wR_factor_ref         0.3340
_reflns_number_gt                9980
_reflns_number_total             14097
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt52552j.txt
_cod_data_source_block           24
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        6004(2)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7029125