NH NMR Shifts of New Structurally Characterized fac-[Re(CO)3(polyamine)]n+ Complexes Probed via Outer-Sphere Hydrogen-Bonding Interactions to Anions, Including the Paramagnetic [ReIVBr6]2- Anion
Theshini Perera; Patricia A. Marzilli; Frank R. Fronczek; Luigi G. Marzilli; Inorganic Chemistry 49 (2010) 5560–5572; doi:10.1021/ic100386c

data_4315771
_publ_section_title
;
 NH NMR Shifts of New Structurally Characterized
 fac-[Re(CO)3(polyamine)]n+ Complexes Probed via Outer-Sphere
 Hydrogen-Bonding Interactions to Anions, Including the Paramagnetic
 [ReIVBr6]2- Anion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5560
_journal_page_last               5572
_journal_paper_doi               10.1021/ic100386c
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C12 H25 N4 O3 Re, 2(P F6)'
_chemical_formula_sum            'C12 H25 F12 N4 O3 P2 Re'
_chemical_formula_weight         749.50
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.620(2)
_cell_length_b                   9.5359(5)
_cell_length_c                   7.9455(5)
_cell_measurement_reflns_used    5807
_cell_measurement_temperature    90.0(5)
_cell_measurement_theta_max      35.6
_cell_measurement_theta_min      2.5
_cell_volume                     2244.2(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare  et al., 1999)'
_diffrn_ambient_temperature      90.0(5)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Nonius KappaCCD (with Oxford Cryostream)'
_diffrn_measurement_method       ' \w scans with \k offsets'
_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  0.0162
_diffrn_reflns_av_sigmaI/netI    0.0212
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            89375
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         35.6
_diffrn_reflns_theta_min         2.7
_exptl_absorpt_coefficient_mu    5.680
_exptl_absorpt_correction_T_max  0.600
_exptl_absorpt_correction_T_min  0.396
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.218
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'needle fragment'
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.36
_refine_diff_density_min         -0.860
_refine_diff_density_rms         0.136
_refine_ls_extinction_coef       0.00058(8)
_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   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         5413
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.030
_refine_ls_R_factor_gt           0.023
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0294P)^2^+2.1227P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.054
_refine_ls_wR_factor_ref         0.057
_reflns_number_gt                4742
_reflns_number_total             5413
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic100386c_si_002_5.cif
_cod_data_source_block           Theshini69
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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 
;
_cod_original_sg_symbol_Hall     '-P 2ac 2n '
_cod_original_sg_symbol_H-M      'P n m a '
_cod_database_code               4315771