Fluoridonitrosyl Complexes of Technetium(I) and Technetium(II). Synthesis, Characterization, Reactions, and DFT Calculations.
Balasekaran, Samundeeswari Mariappan; Spandl, Johann; Hagenbach, Adelheid; Köhler, Klaus; Drees, Markus; Abram, Ulrich; Inorganic chemistry 53 (2014) 5117–5128; doi:10.1021/ic500229r

data_4338310
_publ_section_title
;
 Fluoridonitrosyl Complexes of Technetium(I) and Technetium(II).
 Synthesis, Characterization, Reactions, and DFT Calculations.
;
_journal_issue                   10
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5117
_journal_page_last               5128
_journal_paper_doi               10.1021/ic500229r
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'F5 N O Tc, O, 2(Rb)'
_chemical_formula_sum            'F5 N O2 Rb2 Tc'
_chemical_formula_weight         409.95
_chemical_name_common
;
Dirubidium pentafluoronitrosyltechnetate(II) monohydrate
;
_chemical_name_systematic
;
Dirubidium pentafluoronitrosyltechnetate(II) monohydrate
;
_space_group_IT_number           63
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.4690(10)
_cell_length_b                   18.960(3)
_cell_length_c                   6.4920(10)
_cell_measurement_reflns_used    3788
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.51
_cell_measurement_theta_min      5.32
_cell_volume                     796.3(2)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    Diamond
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_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  0.1095
_diffrn_reflns_av_sigmaI/netI    0.0534
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            2951
_diffrn_reflns_theta_full        29.16
_diffrn_reflns_theta_max         29.16
_diffrn_reflns_theta_min         5.33
_exptl_absorpt_coefficient_mu    13.997
_exptl_absorpt_correction_T_max  0.5039
_exptl_absorpt_correction_T_min  0.0782
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
P. Coppens in "Crystallographic Computing" ed F.R Ahmed, S.R. Hall 
and C.P.Huber, Copenhagen, Munksgaard, (1979) pp 255-270
;
_exptl_crystal_colour            blue-violet
_exptl_crystal_density_diffrn    3.420
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             740
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.227
_exptl_crystal_size_min          0.090
_refine_diff_density_max         2.314
_refine_diff_density_min         -1.977
_refine_diff_density_rms         0.308
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     38
_refine_ls_number_reflns         620
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0546
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1072P)^2^+1.2894P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1430
_refine_ls_wR_factor_ref         0.1563
_reflns_number_gt                564
_reflns_number_total             620
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic500229r_si_002.cif
_cod_data_source_block           rb2[tc(no)f5]
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4338309--4338316.cif.
;
_cod_original_sg_symbol_H-M      Cmcm
_cod_database_code               4338310