Complexation of Diphenyl(phenylacetenyl)phosphine to Rhodium(III) Tetraphenyl Porphyrins: Synthesis and Structural, Spectroscopic, and Thermodynamic Studies
Eugen Stulz; Sonya M. Scott; Andrew D. Bond; Sijbren Otto; Jeremy K. M. Sanders; Inorganic Chemistry 42 (2003) 3086–3096; doi:10.1021/ic026257a

data_4313564
_publ_contact_author_address
;
   Department of Chemistry
   University of Cambridge
   Lensfield Road
   Cambridge
   CB2 1EW
   UK
;
_publ_contact_author_email       adb29@cam.ac.uk
_publ_contact_author_fax         '(01223) 336362'
_publ_contact_author_name        'Andrew D. Bond'
_publ_contact_author_phone       '(01223) 336352'
_publ_section_title
;
 Complexation of Diphenyl(phenylacetenyl)phosphine to Rhodium(III)
 Tetraphenyl Porphyrins: Synthesis and Structural, Spectroscopic, and
 Thermodynamic Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3086
_journal_page_last               3096
_journal_paper_doi               10.1021/ic026257a
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         'C65 H46 N4 P Rh'
_chemical_formula_sum            'C65 H46 N4 P Rh'
_chemical_formula_weight         1016.94
_chemical_name_common            (Me)(dpap)Rh(III)TPP
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                83.942(3)
_cell_angle_beta                 86.237(3)
_cell_angle_gamma                89.875(4)
_cell_formula_units_Z            2
_cell_length_a                   13.3949(7)
_cell_length_b                   13.3979(8)
_cell_length_c                   14.1945(9)
_cell_measurement_reflns_used    33665
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      22.46
_cell_measurement_theta_min      1.00
_cell_volume                     2527.7(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius, 1998)'
_computing_data_reduction
;
   HKL Denzo and Scalepack (Otwinowski & Minor, 1997)
;
_computing_publication_material  'SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_structure_solution    'SIR-92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'Thin slice \w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0815
_diffrn_reflns_av_sigmaI/netI    0.0881
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15705
_diffrn_reflns_theta_full        21.97
_diffrn_reflns_theta_max         21.97
_diffrn_reflns_theta_min         3.52
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.416
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav Blessing (1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.01
_refine_diff_density_max         3.586
_refine_diff_density_min         -0.713
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         6127
_refine_ls_number_restraints     178
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.1337
_refine_ls_R_factor_gt           0.1134
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1318P)^2^+30.6877P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2722
_refine_ls_wR_factor_ref         0.2873
_reflns_number_gt                4980
_reflns_number_total             6127
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic026257a_1.cif
_cod_data_source_block           5
_cod_database_code               4313564