Rhodium Complexes with the Chelating and Binucleating Ligands P(CH~2~CH~2~Py)~n~Ph~3-n~, (Py = 2-Pyridyl; n= 1, 2): Structures and Fluxional Behavior
M. Aránzazu Alonso; Juan A. Casares; Pablo Espinet; Katerina Soulantica; Jonathan P. H. Charmant; A. Guy Orpen; Inorganic Chemistry 39 (2000) 705–711; doi:10.1021/ic990634a

data_4300055
_publ_contact_author
;
 Dr Jonathan P. H. Charmant
 School of Chemistry
 University of Bristol
 Bristol
 BS8 1TS
 UK
;
_publ_contact_author_email       jon.charmant@bris.ac.uk
_publ_contact_author_fax         '+44(0)117 929 0509'
_publ_contact_author_phone       '+44(0)117 928 9812'
_publ_section_title
;
Rhodium Complexes with the Chelating and Binucleating Ligands
P(CH~2~CH~2~Py)~n~Ph~3-n~, (Py = 2-Pyridyl; n= 1, 2): Structures and Fluxional
Behavior
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              705
_journal_page_last               711
_journal_paper_doi               10.1021/ic990634a
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C28 H31 Cl2 F6 N2 P2 Rh'
_chemical_formula_weight         745.30
_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                 99.658(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.4552(10)
_cell_length_b                   18.0676(32)
_cell_length_c                   19.7286(27)
_cell_measurement_reflns_used    210
_cell_measurement_temperature    173(2)
_cell_volume                     2971.1(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens SMART'
_diffrn_measurement_method       'Frames each covering 0.3 deg in \w'
_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  0.0232
_diffrn_reflns_av_sigmaI/netI    0.0326
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18796
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.54
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    0.923
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_correction_T_min  0.726
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Sheldrick, G.M. SADABS: 
 A program for absorption correction with the Siemens SMART system; 
 University of G\"ottingen, Germany, 1996. 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.435
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.998
_refine_ls_goodness_of_fit_obs   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         6793
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.998
_refine_ls_restrained_S_obs      1.061
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_obs          0.0264
_refine_ls_shift/esd_max         0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0359P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0660
_refine_ls_wR_factor_obs         0.0624
_reflns_number_observed          5468
_reflns_number_total             6793
_reflns_observed_criterion       >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0359P)^2^+0.0000P] 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^)+(0.0359P)^2^+0.0000P] 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        2971.13(81)
_cod_database_code               4300055