Ru and Os Complexes Containing a P,N-Donor Heterotopic Ligand: The Effect of Solvent on Stereochemistry
Dabb, Serin L.; Messerle, Barbara A.; Smith, Matthew K.; Willis, Anthony C.; Inorganic Chemistry 47 (2008) 3034–3044; doi:10.1021/ic7019044

data_4304400
_publ_section_title
;
 Ru and Os Complexes Containing a P,N-Donor Heterotopic Ligand:
 The Effect of Solvent on Stereochemistry
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   8
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3034
_journal_page_last               3044
_journal_paper_doi               10.1021/ic7019044
_journal_volume                  47
_journal_year                    2008
_chemical_compound_source        'from UNSW'
_chemical_formula_moiety
;
    C68 H68 Cl2 N8 Os2 P4 2+, 2(C24 H20 B -), 4(C3 H6 O)
;
_chemical_formula_sum            'C128 H132 B2 Cl2 N8 O4 Os2 P4'
_chemical_formula_weight         2443.33
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             06-12-04
_audit_creation_method           CRYSTALS_ver_12.18
_audit_update_record
;
2006-12-04 - Report on C128 H132 B2 Cl2 N8 O4 Os2 P4
             by Anthony C. Willis
             for   Serin Dabb and Barbara Messerle (UNSW)

2006-12-05 - passes checkcif tests with minor warnings

;
_cell_angle_alpha                90
_cell_angle_beta                 97.2536(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.4958(1)
_cell_length_b                   30.2710(2)
_cell_length_c                   20.4361(2)
_cell_measurement_reflns_used    221892
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.6
_cell_volume                     11350.32(15)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius BV, 1997)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
; 
ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
;
_computing_publication_material  'CRYSTALS (Watkin et al 2003)'
_computing_structure_refinement  'CRYSTALS (Watkin et al 2003)'
_computing_structure_solution    'SIR92 (Altomare et al, 1994)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       ' \f and \w scans with CCD '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.059
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            191655
_diffrn_reflns_theta_full        27.476
_diffrn_reflns_theta_max         27.476
_diffrn_reflns_theta_min         2.553
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.398
_exptl_absorpt_correction_T_max  0.683
_exptl_absorpt_correction_T_min  0.435
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             4976
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.19
_refine_diff_density_min         -1.00
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9562
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1344
_refine_ls_number_reflns         25915
_refine_ls_number_restraints     22
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0242
_refine_ls_shift/su_max          0.09
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, Chebychev polynomial, (Watkin, 1994, Prince, 1982). 

  w = [1-(F~o~ - F~c~)^2^/36\s^2^(F)]^2^/ 
 [19.0T~0~(x) + 28.3T~1~(x) + 16.1T~2~(x) + 6.33T~3~(x) + 0.829T~4~(x)]

 where T~i~ are the Chebychev polynomials and x = F~c~/F~max~
(Watkin, 1994, Prince, 1982)

;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0733
_refine_ls_wR_factor_gt          0.0561
_refine_ls_wR_factor_ref         0.0733
_reflns_limit_h_max              23
_reflns_limit_h_min              -24
_reflns_limit_k_max              39
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                18018
_reflns_number_total             25984
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.90
_oxford_diffrn_Wilson_scale      148.16
_oxford_refine_ls_scale          0.108756(11)
_oxford_structure_analysis_title '11301147 nsw0612'
_cod_data_source_file            ic7019044-file006.cif
_cod_data_source_block           nsw0612
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 
;
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4304400