Guanidinates as chelating anionic ligands for early, middle and late transition metals: syntheses and crystal structures of [Ti{η2-(NPh)2CNEt2}2Cl2], [Ru{η2-(NPh)2CNHPh}3] and [Pt{η2-(NPh)2CNHPh}2]
Bailey, Philip J.; Grant, Keith J.; Mitchell, Lindsey A.; Pace, Stuart; Parkin, Andrew; Parsons, Simon; Journal of the Chemical Society, Dalton Transactions  (2000) 1887–; doi:10.1039/b001992p

data_7009569
_publ_section_title
;
 Guanidinates as chelating anionic ligands for early, middle and late
 transition metals: syntheses and crystal structures of
 [Ti{\h2-(NPh)2CNEt2}2Cl2], [Ru{\h2-(NPh)2CNHPh}3] and
 [Pt{\h2-(NPh)2CNHPh}2]
;
_journal_issue                   12
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1887
_journal_paper_doi               10.1039/b001992p
_journal_year                    2000
_chemical_formula_sum            'C62 H60 N9 Ru'
_chemical_formula_weight         1032.26
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.248(3)
_cell_length_b                   20.648(4)
_cell_length_c                   11.784(2)
_cell_measurement_temperature    150(2)
_cell_volume                     5413.3(16)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measurement_method       omega-theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1011
_diffrn_reflns_av_sigmaI/netI    0.0854
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5089
_diffrn_reflns_theta_max         60.03
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    2.710
_exptl_absorpt_correction_T_max  0.412
_exptl_absorpt_correction_T_min  0.469
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_description       needle
_exptl_crystal_F_000             2156
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.447
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.043
_refine_ls_goodness_of_fit_obs   1.034
_refine_ls_matrix_type           full
_refine_ls_number_parameters     644
_refine_ls_number_reflns         4167
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.098
_refine_ls_restrained_S_obs      1.035
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_obs          0.0544
_refine_ls_shift/esd_max         0.041
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0369P)^2^+10.5681P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1358
_refine_ls_wR_factor_obs         0.1096
_reflns_number_observed          3237
_reflns_number_total             4193
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b001992p.txt
_cod_data_source_block           capgwa
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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:

'_exptl_absorpt_correction_type' tag value 'Psi-scans' was replaced
with 'psi-scan' value.

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^)+(0.0369P)^2^+10.5681P] where 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^)+(0.0369P)^2^+10.5681P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      Pna2(1)
_cod_database_code               7009569