Structure of (2,4-pentanedionato-<i>O</i>,<i>O</i>')bis(phenyl 3,3',5,5'-tetra-<i>tert</i>-butyl-1,1'-biphenyl-2,2'-diyl phosphite-<i>P</i>)rhodium
Meetsma, A.; Jongsma, T.; Challa, G.; van Leeuwen, P. W. N. M.; Acta Crystallographica Section C 49 (1993) 1160–1163; doi:10.1107/S0108270192013246

data_2001620
_publ_contact_author
;
     Meetsma, Auke
     Crystal Structure Center
     Department of Chemical Physics
     University of Groningen
     Nijenborgh 4
     NL-9747 AG Groningen
     The Netherlands
;
_publ_section_title
;
 Structure of (2,4-pentanedionato-<i>O</i>,<i>O</i>')bis(phenyl
 3,3',5,5'-tetra-<i>tert</i>-butyl-1,1'-biphenyl-2,2'-diyl
 phosphite-<i>P</i>)rhodium
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1160
_journal_page_last               1163
_journal_paper_doi               10.1107/S0108270192013246
_journal_volume                  49
_journal_year                    1993
_chemical_formula_moiety         'C73 H97 O8 P2 Rh,2(C7 H8)'
_chemical_formula_sum            'C87 H113 O8 P2 Rh'
_chemical_formula_weight         1359.56
_chemical_name_systematic
;
(2,4-Pentanedionato-O,O')bis(phenyl
3,3',5,5'-tetra-tert-butyl-1,1'-biphenyl-2,2'-diyl phosphite-P)rhodium
;
_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_type_scat_source
;Cromer & Mann (1968) [anomalous-dispersion factors from Cromer &
Liberman (1970)]
;
_audit_creation_method
;
     spawned by the program PLATON with option: TABLE ACC
;
_cell_angle_alpha                79.884(8)
_cell_angle_beta                 84.812(6)
_cell_angle_gamma                75.398(9)
_cell_formula_units_Z            2
_cell_length_a                   11.6240(10)
_cell_length_b                   17.244(2)
_cell_length_c                   18.8770(10)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    130
_cell_measurement_theta_max      18.83
_cell_measurement_theta_min      14.84
_cell_volume                     3600.4(6)
_computing_cell_refinement
;
   CAD4, version 5.0, SET4 (de Boer & Duisenberg, 1984)
;
_computing_data_collection       'CAD4, version 5.0 (Enraf-Nonius, 1988)'
_computing_data_reduction        'EUCLID package (Spek, 1982)'
_computing_molecular_graphics    'PLUTO92 (Meetsma, 1992)'
_computing_publication_material  'PLATON92 (Spek, 1992)'
_computing_structure_refinement  'XTAL_CRYLSQ (Olthof, 1990)'
_computing_structure_solution    'SHELXS (Sheldrick, 1990)'
_diffrn_ambient_temperature      130
_diffrn_measurement_device
;
    Enraf-Nonius CAD-4F  single-crystal
;
_diffrn_measurement_method       ' \w/2\q'
_diffrn_radiation_monochromator  'perpendicular mounted graphite'
_diffrn_radiation_source         'fine focus Philips Mo tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.022
_diffrn_reflns_av_sigmaI/netI    0.040
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14851
_diffrn_reflns_reduction_process
;Intensity data were corrected for Lorentz and polarization effects and the
 scale variation, but not for absorption. Standard deviations in the
 intensities based on counting statistics were increased according to an
 analysis of the excess variance (McCandlish, Stout & Andrews, 1975) of the
 three reference reflections: \s^2^(I) = \s^2^~cs~(I) + (0.027I)^2^.
 Equivalent reflections were averaged, resulting in 10706 reflections
 satisfying the I > 2.5\s(I) criterion of observability.
;
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.10
_diffrn_standards_decay_%        0.3
_diffrn_standards_interval_time  180
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.328
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.99
_refine_diff_density_min         0.92
_refine_ls_abs_structure_details ?
_refine_ls_extinction_coef       0.63(9)x10^-4^
_refine_ls_extinction_method     'Zachariasen (1967)'
_refine_ls_goodness_of_fit_obs   1.842
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1136
_refine_ls_number_reflns         10706
_refine_ls_R_factor_obs          0.042
_refine_ls_shift/esd_max         0.77
_refine_ls_shift/esd_mean        0.01
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(F)]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.046
_refine_ls_wR_factor_obs         0.046
_reflns_number_observed          10706
_reflns_number_total             14851
_reflns_observed_criterion       refl_observed_if_I_>_2.5_sigma(I)
_cod_data_source_file            ab1032.cif
_cod_data_source_block           CP178
_cod_depositor_comments
;
 Changing the _atom_site_occupancy data item value from '.' to '1'
 for all fully occupied atom sites.

 Antanas Vaitkus,
 2017-02-10

The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w = 1/[\s^2^(F)]' 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^(F)]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               2001620