Technetium(V) and rhenium(V) complexes of biguanide derivatives. Crystal structures
Marchi, Andrea; Marvelli, Lorenza; Cattabriga, Michela; Rossi, Roberto; Neves, Maria; Bertolasi, Valerio; Ferretti, Valeria; Journal of the Chemical Society, Dalton Transactions  (1999) 1937–; doi:10.1039/a900798i

data_7027290
_publ_section_title
;
 Technetium(V) and rhenium(V) complexes of biguanide derivatives. Crystal
 structures
;
_journal_issue                   12
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1937
_journal_paper_doi               10.1039/a900798i
_journal_year                    1999
_chemical_compound_source        ?
_chemical_formula_analytical     'C33 H44 B1 N10 O2 Tc1'
_chemical_formula_moiety         '[C8 H20 N10 O1 Tc1]+.[C24 H20 B1]-.C1 H4 O1'
_chemical_formula_sum            'C33 H44 B N10 O2 Tc'
_chemical_formula_weight         722.49
_chemical_name_systematic        ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   Fourier
_cell_angle_alpha                90.00(0)
_cell_angle_beta                 96.97(1)
_cell_angle_gamma                90.00(0)
_cell_formula_units_Z            4.00
_cell_length_a                   11.589(2)
_cell_length_b                   15.918(2)
_cell_length_c                   18.962(4)
_cell_measurement_radiation      'Mo K\a'
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_measurement_wavelength     0.71069
_cell_volume                     3472.1(10)
_diffrn_ambient_temperature      295
_diffrn_measurement_device_type  'Enraf-Nonius CAD4 diffractometer'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.028
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7792
_diffrn_reflns_reduction_process ?
_diffrn_reflns_theta_max         27
_diffrn_reflns_theta_min         2
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.4602
_exptl_absorpt_correction_T_max  1.
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '[North, Phillips & Mathews, 1968]'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.3821
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1504.0
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.043
_refine_diff_density_min         -0.035
_refine_ls_abs_structure_details ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.23
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     558
_refine_ls_number_reflns         6172
_refine_ls_R_factor_gt           0.042
_refine_ls_shift/su_max          0.02
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w= 4F^2^/(\s^2^(I) + (0.04F^2^)^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.062
_reflns_number_gt                6172
_reflns_number_total             7561
_reflns_threshold_expression     I>3sima(I)
_cod_data_source_file            900798isup1.cif
_cod_data_source_block           (II)
_cod_depositor_comments
;
 Changing the _atom_site_occupancy data item value from '.' to '1'
 for all fully occupied atom sites.

 Antanas Vaitkus,
 2017-02-10

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w= 4F^2^/(\s^2^(I) +
(0.04F^2^)^2^)' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w= 4F^2^/(\s^2^(I) + (0.04F^2^)^2^)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3472.(1)
_cod_original_sg_symbol_H-M      ' P21/c         '
_cod_original_formula_sum        ' C33 H44 B1 N10 O2 Tc1 '
_cod_database_code               7027290