Octahedral Alkynylphosphine Ruthenium(II) Complexes: Synthesis, Structure, and Electrochemistry
Berenguer, Jesús; Bernechea, María; Fernández, Julio; Gil, Belén; Lalinde, Elena; Moreno, M. Teresa; Ruiz, Santiago; Sánchez, Sergio; Organometallics 30 (2011) 4665–; doi:10.1021/om2005194

data_4065029
_publ_section_title
;
 Octahedral Alkynylphosphine Ruthenium(II) Complexes: Synthesis,
 Structure, and Electrochemistry
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4665
_journal_paper_doi               10.1021/om2005194
_journal_volume                  30
_journal_year                    2011
_chemical_absolute_configuration ad
_chemical_formula_sum            'C126 H116 Cl6 Fe4 P4 Ru'
_chemical_formula_weight         2291.37
_chemical_name_common            'Compound X'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2011-02-10T09:29:26-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            2
_cell_length_a                   15.310(5)
_cell_length_b                   15.310(5)
_cell_length_c                   23.666(5)
_cell_measurement_reflns_used    7728
_cell_measurement_temperature    130.0(10)
_cell_volume                     5547(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      130.0(10)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.0452196
_diffrn_orient_matrix_UB_12      -0.0272508
_diffrn_orient_matrix_UB_13      -0.0248788
_diffrn_orient_matrix_UB_21      0.0356345
_diffrn_orient_matrix_UB_22      -0.0151172
_diffrn_orient_matrix_UB_23      0.0340357
_diffrn_orient_matrix_UB_31      -0.0308507
_diffrn_orient_matrix_UB_32      -0.0574043
_diffrn_orient_matrix_UB_33      0.0028472
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0697
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            35784
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    0.89
_exptl_absorpt_correction_T_max  0.719
_exptl_absorpt_correction_T_min  0.577
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        multi-scan from symmetry-related measurements
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2164
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.45
_platon_squeeze_details
;
platon (Spek 1995)
;
_refine_diff_density_max         2.22
_refine_diff_density_min         -0.798
_refine_diff_density_rms         0.253
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.10(4)
_refine_ls_extinction_coef       0.0163(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_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         6294
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0854
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1419P)^2^+14.0580P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2166
_refine_ls_wR_factor_ref         0.2212
_reflns_number_gt                5812
_reflns_number_total             6294
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om2005194_si_001.cif
_cod_data_source_block           trans-7a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'contr' was replaced with the
value 'constr' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_database_code               4065029