Bond catastrophes in rhodium complexes: experimental charge-density studies of [Rh(C~7~H~8~)(P^<i>t^</i>Bu~3~)Cl] and [Rh(C~7~H~8~)(PCy~3~)Cl]
Sparkes, Hazel A.; Chaplin, Adrian B.; Weller, Andrew S.; Howard, Judith A. K.; Acta Crystallographica Section B 66 (2010) 503–514; doi:10.1107/S0108768110031496

data_2017784
_publ_section_title
;
 Bond catastrophes in rhodium complexes: experimental charge-density
 studies of [Rh(C~7~H~8~)(P^<i>t^</i>Bu~3~)Cl] and
 [Rh(C~7~H~8~)(PCy~3~)Cl]
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              503
_journal_page_last               514
_journal_paper_doi               10.1107/S0108768110031496
_journal_volume                  66
_journal_year                    2010
_chemical_formula_moiety         'C25 H41 Cl P Rh'
_chemical_formula_sum            'C25 H41 Cl P Rh'
_chemical_formula_weight         510.91
_chemical_name_systematic
; 
 ? 
;
_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_type_scat_source
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.0
_cell_angle_beta                 97.7784(6)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   10.21309(7)
_cell_length_b                   15.82275(8)
_cell_length_c                   14.64123(8)
_cell_measurement_reflns_used    46899
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      50.4416
_cell_measurement_theta_min      2.5701
_cell_volume                     2344.24(2)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.5 (release 18-04-2008 CrysAlis171 .NET)
(compiled Apr 18 2008,18:17:43)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.5 (release 18-04-2008 CrysAlis171 .NET)
(compiled Apr 18 2008,18:17:43)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.5 (release 18-04-2008 CrysAlis171 .NET)
(compiled Apr 18 2008,18:17:43)
;
_computing_molecular_graphics    'Volkov et al, (2006)'
_computing_publication_material  'Volkov et al, (2006)'
_computing_structure_refinement  'Volkov et al, (2006)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1998)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.1511
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_sigmaI/netI    0.0225
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            297875
_diffrn_reflns_theta_full        48.88
_diffrn_reflns_theta_max         48.883
_diffrn_reflns_theta_min         2.573
_exptl_absorpt_coefficient_mu    0.920
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
Analytical numeric absorption correction using a multifaceted crystal
   model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1072
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.390
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.229
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         18953
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.028
_refine_ls_R_factor_gt           0.016
_refine_ls_R_Fsqd_factor         0.020
_refine_ls_shift/su_max          0
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
calc w1 = 1/[s^2^(Fo)]
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.013
_reflns_number_gt                21046
_reflns_number_total             24737
_reflns_threshold_expression     'I >3 \s(I)'
_cod_data_source_file            so5039.cif
_cod_data_source_block           RhC7H8PCy3Cl
_cod_original_cell_volume        2344.24(5)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2017784
_cod_database_fobs_code          2017784