Synthesis and characterization of ruthenium quinolin-8-olate complexes. Unexpected formation of a κ1-hydrotris(pyrazolyl)borate complex
Gemel, Christian; John, Roland; Slugovc, Christian; Mereiter, Kurt; Schmid, Roland; Kirchner, Karl; Journal of the Chemical Society, Dalton Transactions  (2000) 2607–; doi:10.1039/b002490m

data_7009657
_publ_section_title
;
 Synthesis and characterization of ruthenium quinolin-8-olate
 complexes. Unexpected formation of a \k1-hydrotris(pyrazolyl)borate
 complex
;
_journal_issue                   15
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2607
_journal_paper_doi               10.1039/b002490m
_journal_year                    2000
_chemical_formula_sum            'C19 H20 Cl N O Ru'
_chemical_formula_weight         414.88
_chemical_name_systematic
; 
 chloro-(8-hydroxyquinolinato-N,O)-(eta$6!-p-cymene)-ruthenium(II)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 102.97(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.757(2)
_cell_length_b                   13.287(3)
_cell_length_c                   12.309(2)
_cell_measurement_reflns_used    18
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      16
_cell_volume                     1714.4(6)
_computing_cell_refinement       'LLSQ4 (Mereiter, 1990)'
_computing_data_collection
'Philips PW1100 and SERVER4 (V\"ollenkle, 1990)'
_computing_data_reduction        'PW114 (Mereiter, 1990) and Siemens XPREP'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      300(2)
_diffrn_measurement_device       'Philips PW1100 four circle diffractometer'
_diffrn_measurement_method       omega-2theta-scans
_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  0.0128
_diffrn_reflns_av_sigmaI/netI    0.0201
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3164
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.28
_diffrn_standards_decay_%        0.7
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.074
_exptl_absorpt_correction_T_max  0.80
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_type   sphere
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_description       prism
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.210
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       0.00027(12)
_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_all   1.037
_refine_ls_goodness_of_fit_obs   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         3012
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.091
_refine_ls_restrained_S_obs      1.048
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_obs          0.0202
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0183P)^2^+0.7299P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0483
_refine_ls_wR_factor_obs         0.0431
_reflns_number_observed          2629
_reflns_number_total             3023
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b002490m.txt
_cod_data_source_block           kinx304
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0183P)^2^+0.7299P] 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^)+(0.0183P)^2^+0.7299P] 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      P2(1)/n
_cod_database_code               7009657