Syntheses and structures of novel cyclic and dinuclear organorhodoximes: a homologous series of di- to penta-methylene-bridged complexes ‡
Steinborn, Dirk; Rausch, Mario; Bruhn, Clemens; Schmidt, Harry; Ströhl, Dieter; Journal of the Chemical Society, Dalton Transactions  (1998) 221–; doi:10.1039/a706184f

data_7028061
_publ_contact_author
;
        Prof. Dr. Dirk Steinborn
        Institut f\"ur Anorganische Chemie
        Martin-Luther-Universit\"at Halle-Wittenberg
        Kurt-Mothes-Str. 2
        06120 Halle(Saale)
        Bundesrepublik Deutschland
;
_publ_section_title
;
 Syntheses and structures of novel cyclic and dinuclear organorhodoximes:
 a homologous series of di- to penta-methylene-bridged
 complexes&#x200A;&#x2021;
;
_journal_issue                   2
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              221
_journal_paper_doi               10.1039/a706184f
_journal_year                    1998
_chemical_compound_source        'see text'
_chemical_formula_sum            'C54 H62 N8 O8 P2 Rh2'
_chemical_formula_weight         1218.88
_chemical_melting_point          '215-220 \%C decomp.'
_chemical_name_systematic
; 

\m-ethane-1,2-diyl-bis[bis(dimethylglyoximato-N,N')(triphenylphos
phine)
 rhodium(III)]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 100.278(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.5199(15)
_cell_length_b                   9.931(2)
_cell_length_c                   16.721(3)
_cell_measurement_reflns_used    79
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      40.41
_cell_measurement_theta_min      10.25
_cell_volume                     2699.2(8)
_computing_cell_refinement       'STADI4 ver. 1.05c (STOE, 1996)'
_computing_data_collection       'STADI4 ver. 1.05c (STOE, 1996)'
_computing_data_reduction        'X-red ver. 1.05 (STOE,1996)'
_computing_molecular_graphics    'ORTEPIII (Johnson, C. K., 1997)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'STOE Stadi4 4-circle-diffractometer'
_diffrn_measurement_method       \w/2q
_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  0.0427
_diffrn_reflns_av_sigmaI/netI    0.0505
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8879
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.40
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  1h
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    0.732
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_type   'empirical via \y-scans'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1252
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.456
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       0.00091(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.111
_refine_ls_goodness_of_fit_obs   1.102
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         4732
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.118
_refine_ls_restrained_S_obs      1.102
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_obs          0.0318
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0257P)^2^+1.1243P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0836
_refine_ls_wR_factor_obs         0.0718
_reflns_number_observed          3678
_reflns_number_total             4737
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            f706184asup1.cif
_cod_data_source_block           stadi121
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0257P)^2^+1.1243P] 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^)+(0.0257P)^2^+1.1243P] 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        2699.2(7)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7028061