Secondary Coordination Sphere Effects in Ruthenium(III) Tetraammine Complexes: Role of the Coordinated Water Molecule.
Souza, Maykon L.; Castellano, Eduardo E.; Telser, Joshua; Franco, Douglas W.; Inorganic chemistry 54 (2015) 2067–2080; doi:10.1021/ic5030857

data_4342359
_publ_section_title
;
 Secondary Coordination Sphere Effects in Ruthenium(III) Tetraammine
 Complexes: Role of the Coordinated Water Molecule.
;
_journal_issue                   4
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2067
_journal_page_last               2080
_journal_paper_doi               10.1021/ic5030857
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C6 H21 N5 O Ru, 3(C F3 O3 S), H2 O'
_chemical_formula_sum            'C9 H21 F9 N5 O10 Ru S3'
_chemical_formula_weight         727.56
_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
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2012-06-16T13:13:55-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 111.515(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8184(5)
_cell_length_b                   14.7690(6)
_cell_length_c                   14.6665(5)
_cell_measurement_reflns_used    9644
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.733
_cell_measurement_theta_min      2.546
_cell_volume                     2784.64(18)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.45632E-1
_diffrn_orient_matrix_UB_12      -0.542937E-1
_diffrn_orient_matrix_UB_13      -0.80276E-2
_diffrn_orient_matrix_UB_21      -0.486047E-1
_diffrn_orient_matrix_UB_22      0.36381E-1
_diffrn_orient_matrix_UB_23      0.218276E-1
_diffrn_orient_matrix_UB_31      -0.40077E-1
_diffrn_orient_matrix_UB_32      0.176969E-1
_diffrn_orient_matrix_UB_33      -0.695012E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0579
_diffrn_reflns_av_unetI/netI     0.0494
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18412
_diffrn_reflns_reduction_process
;
 Scaled and merged with Sortav
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        26
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_min         2.89
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.896
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1452
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.061
_refine_diff_density_max         1.747
_refine_diff_density_min         -0.908
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       0.024(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_ref   1.08
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         5429
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0888
_refine_ls_R_factor_gt           0.0695
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1345P)^2^+1.3859P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.195
_refine_ls_wR_factor_ref         0.2115
_reflns_number_gt                4007
_reflns_number_total             5429
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic5030857_si_003.cif
_cod_data_source_block           s93
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

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

 Adding full bibliography for 4342358--4342360.cif.
;
_cod_original_sg_symbol_Hall     -P2yn
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4342359