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_4304398
_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
'C34 H34 Cl2 N4 P2 Ru, 1.5(C H2 Cl2), 0.25(H2 O)'
_chemical_formula_sum            'C35.5 H37.5 Cl5 N4 O0.25 P2 Ru'
_chemical_formula_weight         864.50
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             06-03-09
_audit_creation_method           CRYSTALS_ver_12.18
_audit_update_record
;
2006-03-09 - Report on C35.5 H37 Cl5 N4 O0.25 P2 Ru
             by Anthony C. Willis
             for   Serin Dabb and Barbara Messerle (UNSW)

2006-03-10 - passes checkcif tests with minor warnings

;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.5441(3)
_cell_length_b                   39.6000(6)
_cell_length_c                   10.2814(2)
_cell_measurement_reflns_used    144707
_cell_measurement_temperature    200
_cell_measurement_theta_max      27
_cell_measurement_theta_min      3
_cell_volume                     7550.1(2)
_computing_cell_refinement       'Denzo/Scalepack '
_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 '
_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  0.075
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            87165
_diffrn_reflns_theta_full        27.480
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         2.741
_diffrn_standards_number         0
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_exptl_absorpt_correction_T_min  0.766
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             3516.00
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.96
_refine_diff_density_min         -1.04
_refine_ls_extinction_method     None
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_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         8627
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0270
_refine_ls_shift/su_max          0.003094
_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^/ 
 [10.1T~0~(x) + 14.3T~1~(x) + 7.55T~2~(x) + 2.48T~3~(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         0.0993
_refine_ls_wR_factor_gt          0.0615
_refine_ls_wR_factor_ref         0.0993
_reflns_limit_h_max              24
_reflns_limit_h_min              0
_reflns_limit_k_max              51
_reflns_limit_k_min              0
_reflns_limit_l_max              13
_reflns_limit_l_min              0
_reflns_number_gt                4654
_reflns_number_total             8647
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.11
_oxford_diffrn_Wilson_scale      122.33
_oxford_refine_ls_scale          0.10121(2)
_oxford_structure_analysis_title nsw061
_cod_data_source_file            ic7019044-file004.cif
_cod_data_source_block           nsw061
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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 c c n '
_cod_database_code               4304398