Controlling Substitution Chemistry in Ruthenium(II) Systems. Synthesis of Heteroleptic Complexes Incorporating the [Ru([9]aneS3)]2+ Metal Center
Sue Roche; Harry Adams; Sharon E. Spey; James A. Thomas; Inorganic Chemistry 39 (2000) 2385–2390; doi:10.1021/ic991336g

data_4320983
_publ_section_title
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 Controlling Substitution Chemistry in Ruthenium(II) Systems. Synthesis of
 Heteroleptic Complexes Incorporating the [Ru([9]aneS3)]2+ Metal Center
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2385
_journal_page_last               2390
_journal_paper_doi               10.1021/ic991336g
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C15 H23 F12 N3 P2 Ru S3'
_chemical_formula_weight         732.55
_chemical_name_systematic
; 
 ? 
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_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.748(5)
_cell_length_b                   18.037(7)
_cell_length_c                   10.341(4)
_cell_measurement_reflns_used    34
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.556
_cell_measurement_theta_min      6.992
_cell_volume                     2750.8(18)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_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  0.0291
_diffrn_reflns_av_sigmaI/netI    0.0372
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            3284
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.78
_diffrn_standards_decay_%        19.17
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.006
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.511
_exptl_absorpt_correction_type   'psi scans'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.769
_exptl_crystal_description       'oblong block'
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.848
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(11)
_refine_ls_extinction_coef       0.0000(3)
_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   1.031
_refine_ls_goodness_of_fit_obs   1.064
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         2848
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.030
_refine_ls_restrained_S_obs      1.063
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_obs          0.0448
_refine_ls_shift/esd_max         -0.458
_refine_ls_shift/esd_mean        0.017
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0863P)^2^+1.2499P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1292
_refine_ls_wR_factor_obs         0.1186
_reflns_number_observed          2320
_reflns_number_total             2848
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic991336g_2.cif
_cod_data_source_block           isn-742
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0863P)^2^+1.2499P] 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^)+(0.0863P)^2^+1.2499P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4320983