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_7010854
_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     'C35 H46 Cl2 N3 O1.50 P Rh'
_chemical_formula_moiety         'C32 H39 Cl2 N3 P Rh.C3 H6 O.[H2 O]0.5'
_chemical_formula_structural     'C35 H46 Cl2 N3 O1.50 P Rh'
_chemical_formula_sum            'C35 H46 Cl2 N3 O1.5 P Rh'
_chemical_formula_weight         737.53
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 91.1350(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.0569(3)
_cell_length_b                   19.4344(5)
_cell_length_c                   13.9166(3)
_cell_measurement_reflns_used    98
_cell_measurement_temperature    566(2)
_cell_measurement_theta_max      168
_cell_measurement_theta_min      12
_cell_volume                     3530.69(14)
_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      566(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  0.0510
_diffrn_reflns_av_sigmaI/netI    0.0619
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14889
_diffrn_reflns_theta_max         23.29
_diffrn_reflns_theta_min         1.80
_diffrn_standards_decay_%        -
_diffrn_standards_interval_count -
_diffrn_standards_interval_time  -
_diffrn_standards_number         -
_exptl_absorpt_coefficient_mu    0.713
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.824253
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    -
_exptl_crystal_description       plate
_exptl_crystal_F_000             1532
_exptl_crystal_size_max          .17
_exptl_crystal_size_mid          .1
_exptl_crystal_size_min          .07
_refine_diff_density_max         1.209
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       0.0006(2)
_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   1.126
_refine_ls_goodness_of_fit_obs   1.220
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         4965
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.363
_refine_ls_restrained_S_obs      1.220
_refine_ls_R_factor_all          0.1009
_refine_ls_R_factor_obs          0.0589
_refine_ls_shift/esd_max         3.158
_refine_ls_shift/esd_mean        0.078
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0812P)^2^+2.1112P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1928
_refine_ls_wR_factor_obs         0.1414
_reflns_number_observed          3382
_reflns_number_total             5036
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b104523g.txt
_cod_data_source_block           11
_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^)+(0.0812P)^2^+2.1112P] 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^)+(0.0812P)^2^+2.1112P] 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        'C35 H46 Cl2 N3 O1.50 P Rh'
_cod_database_code               7010854