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_7028064
_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            'C29 H34 N4 O4 P Rh'
_chemical_formula_weight         636.48
_chemical_melting_point          '170-172 \% C decomp.'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 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                 100.232(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.298(2)
_cell_length_b                   11.928(2)
_cell_length_c                   33.903(5)
_cell_measurement_reflns_used    2000
_cell_measurement_temperature    293(2)
_cell_volume                     6088.0(16)
_computing_cell_refinement
;
 Stoe IPDS-software (STOE publication 4805-010, 1996)
;
_computing_data_collection
;
 Stoe IPDS-software (STOE publication 4805-010, 1996)
;
_computing_data_reduction
;
 Stoe IPDS-software (STOE publication 4805-010, 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 Image Plate Detection System'
_diffrn_measurement_method
;
 The reciprocical space was scanned with 133 images each of which
 with an exposure time of 5 min and a rotation angle of 1.5
degrees.
;
_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  0.1032
_diffrn_reflns_av_sigmaI/netI    0.0595
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            25709
_diffrn_reflns_theta_max         23.97
_diffrn_reflns_theta_min         1.81
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         'max. 50 per image'
_exptl_absorpt_coefficient_mu    0.652
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       plate
_exptl_crystal_F_000             2624
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.199
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.174
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.116
_refine_ls_goodness_of_fit_obs   1.206
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         4725
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.116
_refine_ls_restrained_S_obs      1.206
_refine_ls_R_factor_all          0.0956
_refine_ls_R_factor_obs          0.0649
_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^)+(0.1260P)^2^+46.1524P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2269
_refine_ls_wR_factor_obs         0.2063
_reflns_number_observed          3410
_reflns_number_total             4725
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            f706184dsup1.cif
_cod_data_source_block           ipds114
_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^)+(0.1260P)^2^+46.1524P] 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^)+(0.1260P)^2^+46.1524P] 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        6088.0(15)
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               7028064