Probing hydrogen bond networks in half-sandwich Ru(II) building blocks by a combined 1H DQ CRAMPS solid-state NMR, XRPD, and DFT approach.
Chierotti, Michele R.; Gobetto, Roberto; Nervi, Carlo; Bacchi, Alessia; Pelagatti, Paolo; Colombo, Valentina; Sironi, Angelo; Inorganic chemistry 53 (2014) 139–146; doi:10.1021/ic401762z

data_4337471
_publ_section_title
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 Probing hydrogen bond networks in half-sandwich Ru(II) building blocks by
 a combined 1H DQ CRAMPS solid-state NMR, XRPD, and DFT approach.
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_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              139
_journal_page_last               146
_journal_paper_doi               10.1021/ic401762z
_journal_volume                  53
_journal_year                    2014
_chemical_compound_source        'Phase transition'
_chemical_formula_analytical     'Ru Cl2 (C10 H14) (C6 O2 H5)'
_chemical_formula_moiety         'C16 H19 Cl2 N O2 Ru'
_chemical_formula_structural     'C16 H19 Cl2 N O2 Ru'
_chemical_formula_sum            'C16 H19 Cl2 N O2 Ru'
_chemical_formula_weight         429.29
_chemical_name_systematic
;
[(eta6-p-cymene)Ru(II)Cl2(isonicotinic acid)]
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yab'
_space_group_name_H-M_alt        'P 1 21/a 1'
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_cell_angle_alpha                90
_cell_angle_beta                 95.2747(43)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.9156(19)
_cell_length_b                   15.34138(87)
_cell_length_c                   7.36774(40)
_cell_measurement_temperature    298
_cell_volume                     3479.6(3)
_computing_cell_refinement       TOPAS-R
_computing_publication_material  TOPAS-R
_computing_structure_refinement  TOPAS-R
_computing_structure_solution    TOPAS-R
_diffrn_ambient_temperature      298
_diffrn_detector_type
;
Bruker Lynxeye linear position sensitive detector
;
_diffrn_measurement_device_type  'Bruker AXS D8 Advance'
_diffrn_radiation_monochromator  'nickel filter'
_diffrn_radiation_wavelength     1.54056
_diffrn_source_target            Cu
_diffrn_source_type              'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    10.4
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1728
_pd_char_colour                  yellow
_pd_instr_location               ' ?'
_pd_meas_2theta_range_inc        0.02
_pd_meas_2theta_range_max        90
_pd_meas_2theta_range_min        4
_pd_meas_number_of_points        4301
_pd_meas_scan_method             cont
_pd_proc_2theta_range_inc        0.02
_pd_proc_2theta_range_max        90
_pd_proc_2theta_range_min        4
_pd_proc_ls_background_function  'Chebychev polynomial'
_pd_proc_ls_profile_function     'fundamental parameters approach'
_pd_proc_ls_prof_R_factor        0.040
_pd_proc_ls_prof_wR_expected     0.028
_pd_proc_ls_prof_wR_factor       0.053
_pd_spec_mounting
;
packed powder pellet
;
_pd_spec_mount_mode              reflection
_pd_spec_shape                   flat_sheet
_pd_spec_size_axial              15
_pd_spec_size_equat              20
_pd_spec_size_thick              0.02
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   2.34
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           fullcycle
_refine_ls_shift/su_max          .01
_refine_ls_structure_factor_coef Inet
_refine_ls_weighting_details     'w = 1/[Y~i~]'
_refine_ls_weighting_scheme      calc
_cod_data_source_file            ic401762z_si_001.cif
_cod_data_source_block           1gamma
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '1/[Y~i~]' was changed to 'calc'.
New tag '_refine_ls_weighting_details' was created. The value of the
new tag was set to 'w = 1/[Y~i~]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_cell_volume        3479.64(35)
_cod_database_code               4337471