A Controlled NO-Releasing Compound: Synthesis, Molecular Structure, Spectroscopy, Electrochemistry, and Chemical Reactivity of R,R,S,S-trans-[RuCl(NO)(cyclam)]2+ (1,4,8,11-tetraazacyclotetradecane)
D. R. Lang; J. A. Davis; L. G. F. Lopes; A. A. Ferro; L. C. G. Vasconcellos; D. W. Franco; E. Tfouni; A. Wieraszko; M. J. Clarke; Inorganic Chemistry 39 (2000) 2294–2300; doi:10.1021/ic9912979

data_4320977
_publ_contact_author_address
;    
    Eugene F. Merkert Chemistry Center
    Department of Chemistry
    Boston College
    2609 Beacon St.
    Chestnut Hill, MA 02467
    U.S.A
;
_publ_contact_author_email       clarke@bc.edu
_publ_contact_author_fax         '617 552 2705'
_publ_contact_author_name        'Dr. M. J. Clarke'
_publ_contact_author_phone       '617 552 3624'
_publ_section_title
;
 A Controlled NO-Releasing Compound: Synthesis, Molecular Structure,
 Spectroscopy, Electrochemistry, and Chemical Reactivity of
 R,R,S,S-trans-[RuCl(NO)(cyclam)]2+ (1,4,8,11-tetraazacyclotetradecane)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2294
_journal_page_last               2300
_journal_paper_doi               10.1021/ic9912979
_journal_volume                  39
_journal_year                    2000
_chemical_formula_moiety         'C8.57 H17.14 Cl2.57 N4.28 O7.71 Ru0.86'
_chemical_formula_sum            'C8.57 H17.14 Cl2.57 N4.28 O7.71 Ru0.86'
_chemical_formula_weight         481.50
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 95.2550(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            7
_cell_length_a                   7.665
_cell_length_b                   24.72440(10)
_cell_length_c                   16.2871(2)
_cell_measurement_reflns_used    129
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      56.68
_cell_measurement_theta_min      3
_cell_volume                     3073.64(4)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_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      183(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  0.1165
_diffrn_reflns_av_sigmaI/netI    0.0705
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18329
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         1.50
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.209
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.821
_exptl_crystal_description       block
_exptl_crystal_F_000             1692
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.135
_refine_diff_density_min         -1.204
_refine_diff_density_rms         0.195
_refine_ls_extinction_coef       0.0018(2)
_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   1.211
_refine_ls_goodness_of_fit_obs   1.218
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         7048
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.217
_refine_ls_restrained_S_obs      1.218
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_obs          0.0575
_refine_ls_shift/esd_mean        0.022
_refine_ls_shift/su_max          -0.333
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0431P)^2^+6.2540P] P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1518
_refine_ls_wR_factor_obs         0.1468
_reflns_number_observed          6591
_reflns_number_total             7049
_reflns_observed_criterion       >2\s(I)
_cod_data_source_file            ic9912979.cif
_cod_data_source_block           ClarkeRuNO
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0431P)^2^+6.2540P] 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^)+(0.0431P)^2^+6.2540P] 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        3073.48(4)
_cod_database_code               4320977