Synthesis and Reactivity of Fluoro Complexes. Part 1. Cyclooctadiene Rhodium(I) Complexes
José Vicente; Juan Gil-Rubio; Delia Bautista; Inorganic Chemistry 40 (2001) 2636–2637; doi:10.1021/ic015526e

data_4319803
_publ_contact_author
; 
 Jose Vicente
Grupo de Quimica Organometalica. Departamento
de Quimica Inorganica, Facultad de Quimica
Universidad de Murcia, apartado 4021
Murcia 30071. Spain
;
_publ_contact_author_email       jvs@um.es
_publ_section_title
;
 Synthesis and Reactivity of Fluoro Complexes. Part 1. Cyclooctadiene
 Rhodium(I) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2636
_journal_page_last               2637
_journal_paper_doi               10.1021/ic015526e
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C27 H27 F3 P Rh'
_chemical_formula_weight         542.37
_chemical_name_systematic
; 
 ? 
;
_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     patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                92.237(5)
_cell_angle_beta                 99.544(4)
_cell_angle_gamma                90.658(4)
_cell_formula_units_Z            4
_cell_length_a                   11.8239(5)
_cell_length_b                   13.0316(7)
_cell_length_c                   15.0851(9)
_cell_measurement_reflns_used    98
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.46
_cell_measurement_theta_min      4.73
_cell_volume                     2290.1(2)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       \w-scans
_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  0.0145
_diffrn_reflns_av_sigmaI/netI    0.0216
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11116
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.10
_diffrn_standards_decay_%        1.1
_diffrn_standards_interval_count 247
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.853
_exptl_absorpt_correction_T_max  0.78749
_exptl_absorpt_correction_T_min  0.75721
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_description       block
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.34
_refine_diff_density_max         0.318
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.066
_refine_ls_goodness_of_fit_obs   1.127
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         8040
_refine_ls_number_restraints     508
_refine_ls_restrained_S_all      1.033
_refine_ls_restrained_S_obs      1.086
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_obs          0.0211
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0252P)^2^+0.7895P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0520
_refine_ls_wR_factor_obs         0.0507
_reflns_number_observed          6931
_reflns_number_total             8040
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic015526e_s2_1.cif
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' tag value 'Psi-scans' was replaced
with 'psi-scan' value.

'_symmetry_cell_setting' value 'Triclinic'
changed to 'triclinic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0252P)^2^+0.7895P] 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^)+(0.0252P)^2^+0.7895P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4319803