Synthesis and structure of novel rhodium complexes of multi-functionalised amine-phosphine ligands
Clarke, Matthew L.; Slawin, Alexandra M. Z.; Wheatley, Matthew V.; Woollins, J. Derek; Journal of the Chemical Society, Dalton Transactions  (2001) 3421–; doi:10.1039/b104523g

data_7010855
_publ_section_title
;
 Synthesis and structure of novel rhodium complexes of
 multi-functionalised amine-phosphine ligands
;
_journal_issue                   23
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3421
_journal_paper_doi               10.1039/b104523g
_journal_year                    2001
_chemical_formula_analytical     'C27.50 H30 Cl3 N O4 P Rh'
_chemical_formula_moiety         'C27 H29 Cl N P Rh.Cl O4.[C H2 Cl2]0.5'
_chemical_formula_structural     'C27.50 H30 Cl3 N O4 P Rh'
_chemical_formula_sum            'C27.5 H30 Cl3 N O4 P Rh'
_chemical_formula_weight         678.76
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 102.928(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   32.668(2)
_cell_length_b                   8.1102(5)
_cell_length_c                   24.401(2)
_cell_measurement_reflns_used    83
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      168
_cell_measurement_theta_min      12
_cell_volume                     6301.0(8)
_computing_cell_refinement       SMART/SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       SMART
_diffrn_measurement_method       CCD
_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  0.0542
_diffrn_reflns_av_sigmaI/netI    0.0602
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            13306
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        -
_diffrn_standards_interval_count -
_diffrn_standards_interval_time  -
_diffrn_standards_number         -
_exptl_absorpt_coefficient_mu    0.878
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.758386
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    -
_exptl_crystal_description       plate
_exptl_crystal_F_000             2760
_exptl_crystal_size_max          .1
_exptl_crystal_size_mid          .1
_exptl_crystal_size_min          .05
_refine_diff_density_max         1.147
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.104
_refine_ls_extinction_coef       0.00000(9)
_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_all   0.868
_refine_ls_goodness_of_fit_obs   0.898
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         4465
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.207
_refine_ls_restrained_S_obs      0.898
_refine_ls_R_factor_all          0.1026
_refine_ls_R_factor_obs          0.0574
_refine_ls_shift/esd_max         -0.721
_refine_ls_shift/esd_mean        0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1285P)^2^+13.4522P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2421
_refine_ls_wR_factor_obs         0.1460
_reflns_number_observed          2931
_reflns_number_total             4515
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b104523g.txt
_cod_data_source_block           13
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value '-' 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^)+(0.1285P)^2^+13.4522P] 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^)+(0.1285P)^2^+13.4522P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        6300.9(7)
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C27.50 H30 Cl3 N O4 P Rh'
_cod_database_code               7010855