Functionalized cyclopentadienyl rhodium(III) bipyridine complexes: synthesis, characterization, and catalytic application in hydrogenation of ketones.
Wang, Wan-Hui; Suna, Yuki; Himeda, Yuichiro; Muckerman, James T.; Fujita, Etsuko; Dalton transactions (Cambridge, England : 2003) 42 (2013) 9628–9636; doi:10.1039/c3dt50445j

data_7022974
_publ_section_title
;
 Functionalized cyclopentadienyl rhodium(III) bipyridine complexes:
 synthesis, characterization, and catalytic application in hydrogenation
 of ketones.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9628
_journal_page_last               9636
_journal_paper_doi               10.1039/c3dt50445j
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C24 H27 Br1 Cl1 N2 O7 Rh1'
_chemical_formula_sum            'C24 H27 Br Cl N2 O7 Rh'
_chemical_formula_weight         673.75
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             05-11-07
_audit_creation_method           CRYSTALS_ver_12.82
_cell_angle_alpha                90
_cell_angle_beta                 95.7930(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9471(8)
_cell_length_b                   10.5506(6)
_cell_length_c                   16.8312(10)
_cell_measurement_reflns_used    3763
_cell_measurement_temperature    293
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      1
_cell_volume                     2640.7(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type  Unknown
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.025
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16362
_diffrn_reflns_theta_full        26.246
_diffrn_reflns_theta_max         28.221
_diffrn_reflns_theta_min         1.369
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.307
_exptl_absorpt_correction_T_max  0.616
_exptl_absorpt_correction_T_min  0.502
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_description       block
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.75
_refine_diff_density_min         -0.60
_refine_ls_extinction_coef       33(14)
_refine_ls_extinction_method
'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_ref   1.0887
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         3763
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.000609
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
1.29 0.680 0.986
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0583
_refine_ls_wR_factor_gt          0.0429
_refine_ls_wR_factor_ref         0.0429
_reflns_limit_h_max              19
_reflns_limit_h_min              -19
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                3763
_reflns_number_total             6050
_reflns_threshold_expression     I>3.00u(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          0.2446(5)
_oxford_structure_analysis_title 'yhrh206 in P2(1)/c'
_cod_data_source_file            c3dt50445j.cif
_cod_data_source_block           CRYSTALS_cif
_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 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C24 H27 Br1 Cl1 N2 O7 Rh1'
_cod_database_code               7022974