Synthesis, Structure, and Reactivity of New Tetranuclear Ru-Hbpp-Based Water-Oxidation Catalysts
Laia Francàs; Xavier Sala; Eduardo Escudero-Adán; Jordi Benet-Buchholz; Lluís Escriche; Antoni Llobet; Inorganic Chemistry 50 (2011) 2771–2781; doi:10.1021/ic101802y

data_4324745
_publ_section_title
;
 Synthesis, Structure, and Reactivity of New Tetranuclear Ru-Hbpp-Based
 Water-Oxidation Catalysts
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2771
_journal_page_last               2781
_journal_paper_doi               10.1021/ic101802y
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C52 H40 F12 N10 O2 P2 Ru2'
_chemical_formula_weight         1329.02
_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                90.713(3)
_cell_angle_beta                 111.643(3)
_cell_angle_gamma                91.573(3)
_cell_formula_units_Z            2
_cell_length_a                   12.6872(7)
_cell_length_b                   14.1522(10)
_cell_length_c                   17.0548(10)
_cell_measurement_reflns_used    2856
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.76
_cell_measurement_theta_min      2.89
_cell_volume                     2844.4(3)
_computing_cell_refinement       'Bruker APEX2 v2009.1-0'
_computing_data_collection       'Bruker APEX2 v2009.1-0'
_computing_data_reduction        'Bruker SAINT V7.60A'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_detector_type            '4K CCD area detector APEX II'
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.882
_diffrn_measurement_device_type  'Kappa 4-axis goniometer bruker-nonius'
_diffrn_measurement_method
;
 Fullsphere data collection, phi and omega scans
;
_diffrn_measurement_specimen_support
'magnetic support whith 10 micron nylon fiber cryoloop'
_diffrn_radiation_monochromator  'Multilayer Montel 200 mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0792
_diffrn_reflns_av_sigmaI/netI    0.1387
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27489
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.49
_diffrn_reflns_theta_min         2.57
_diffrn_source                   'rotating anode X-ray tube'
_diffrn_source_current           70
_diffrn_source_power             50
_diffrn_source_size              '3 mm x 0.3 mm fine focus'
_diffrn_source_type              'Bruker-Nonius FR 591'
_exptl_absorpt_coefficient_mu    0.675
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.99
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 SADABS Version 2008/1 Bruker-Nonius
 Blessing, Acta Cryst. (1995) A51 33-38
;
_exptl_crystal_colour            translucent
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_description       plate
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_platon_squeeze_details
;
 The programm SQUEEZE implemented in Platon was used to avoid
 highly disordered methanol molecules. Platon Reference: A.L.Spek
 (1990) Acta. Cryst. A46, C34. PLATON - A multipurpose
 Crystallgraphic Tool Utrech University, Utrecht, The Netherlands.
 A. L. Speck (2006). For Squeeze: P. van der Sluis & A.L. Spek
 (1990). Acta Cryst. A46, 194-201).
;
_refine_diff_density_max         1.154
_refine_diff_density_min         -1.130
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1088
_refine_ls_number_reflns         13968
_refine_ls_number_restraints     1753
_refine_ls_restrained_S_all      0.920
_refine_ls_R_factor_all          0.1410
_refine_ls_R_factor_gt           0.0724
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0996P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1700
_refine_ls_wR_factor_ref         0.1937
_reflns_number_gt                7482
_reflns_number_total             13968
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101802y_si_003.cif
_cod_data_source_block           lff10310a_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '_diffrn_measurement_specimen_suppport' was replaced with
'_diffrn_measurement_specimen_support' as specified in the
replacement file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
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_cod_database_code               4324745