Tetraethylammonium tricarbonylchlorido(isoquinoline-1-carboxylato-κ^2^<i>N</i>,<i>O</i>)technetate(I)
Schmalle, Helmut W.; Alberto, Roger; Acta Crystallographica Section E 64 (2008) m1213–m1214; doi:10.1107/S160053680802713X

data_2219352
_publ_section_title
;Tetraethylammonium
 tricarbonylchlorido(isoquinoline-1-carboxylato-\k^2^<i>N</i>,<i>O</i>)technetate(I)
;
_journal_coeditor_code           HB2781
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1213
_journal_page_last               m1214
_journal_paper_doi               10.1107/S160053680802713X
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '(C8 H20 N) [Tc (C10 H6 N O2) Cl (C O)3]'
_chemical_formula_moiety         'C8 H20 N +, C13 H6 Cl N O5 Tc -'
_chemical_formula_sum            'C21 H26 Cl N2 O5 Tc'
_chemical_formula_weight         520.80
_chemical_name_systematic
;
Tetraethylammonium
tricarbonylchlorido(isoquinoline-1-carboxylato-\k^2^N,O)technetate(I)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.878(12)
_cell_angle_beta                 109.624(12)
_cell_angle_gamma                99.052(13)
_cell_formula_units_Z            4
_cell_length_a                   11.7657(14)
_cell_length_b                   12.7481(14)
_cell_length_c                   17.1855(18)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      30.45
_cell_measurement_theta_min      2.3
_cell_volume                     2290.0(5)
_computing_cell_refinement       'IPDS Software (Stoe & Cie, 1997)'
_computing_data_collection       'IPDS Software (Stoe & Cie, 1997)'
_computing_data_reduction        'XRED (Stoe & Cie, 1997)'
_computing_molecular_graphics    'PLATON and PLUTON (Spek, 2003)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.936
_diffrn_measured_fraction_theta_max 0.904
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       '\f rotation scan'
_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  0.0575
_diffrn_reflns_av_sigmaI/netI    0.0271
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            29670
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.33
_diffrn_reflns_theta_min         2.85
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count image
_diffrn_standards_interval_time  4.20
_diffrn_standards_number         '50 to 200'
_exptl_absorpt_coefficient_mu    0.779
_exptl_absorpt_correction_T_max  0.828
_exptl_absorpt_correction_T_min  0.670
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(Coppens <i>et al.</i>,  1965)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular plate'
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.77
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.539
_refine_diff_density_min         -1.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         12462
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0275
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.04P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0650
_refine_ls_wR_factor_ref         0.0668
_reflns_number_gt                9515
_reflns_number_total             12462
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb2781.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2219352
_cod_database_fobs_code          2219352