Bis(acetylacetonato)ruthenium(II) complexes containing alkynyldiphenylphosphines. Formation and redox behaviour of [Ru(acac)2(Ph2PC triple bond CR)2] (R=H, Me, Ph) complexes and the binuclear complex cis-[{Ru(acac)2}2(micro-Ph2PC triple bond CPPh2)}2].
Bennett, Martin A.; Byrnes, Matthew J.; Willis, Anthony C.; Dalton transactions (Cambridge, England : 2003)  (2007) 1677–1686; doi:10.1039/b618365d

data_7005244
_publ_section_title
;
 Bis(acetylacetonato)ruthenium(II) complexes containing
 alkynyldiphenylphosphines. Formation and redox behaviour of
 [Ru(acac)2(Ph2PC triple bond CR)2] (R=H, Me, Ph) complexes and the
 binuclear complex cis-[{Ru(acac)2}2(micro-Ph2PC triple bond CPPh2)}2].
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1677
_journal_page_last               1686
_journal_paper_doi               10.1039/b618365d
_journal_year                    2007
_chemical_compound_source        local
_chemical_formula_moiety         'C72 H68 O8 P4 Ru2, 0.5(C H2 Cl2), 0.5(C6 H14)'
_chemical_formula_sum            'C75.5 H76 Cl O8 P4 Ru2'
_chemical_formula_weight         1472.92
_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
_audit_creation_date             06-09-18
_audit_creation_method           CRYSTALS_ver_12.18
_audit_update_record
;
2000-04 acw tries to model solvent area with sensible fragments -
but gets nowhere.
2000-04-13 acw puts together a cif for mjb's thesis with solvent area
as unidentified atoms.
2006-09-19 acw tidies up structure using CRYSTALS
;
_cell_angle_alpha                90
_cell_angle_beta                 102.41(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.096(4)
_cell_length_b                   22.508(4)
_cell_length_c                   27.778(3)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    193.2
_cell_measurement_theta_max      54.8
_cell_measurement_theta_min      53.9
_cell_volume                     7386(3)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1992-1997)'
_computing_molecular_graphics
;
ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
;
_computing_publication_material  'CRYSTALS (Watkin et al 2003)'
_computing_structure_refinement  'CRYSTALS (Watkin et al 2003)'
_computing_structure_solution    'SIR92 (Altomare et al, 1994)'
_diffrn_ambient_temperature      193.2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_details
;
Rigaku AFC6R diffractometer with extended arm and
evacuated collimator and beam tunnel.
Data cannot be collected beyond \y 60 deg in this configuration.
;
_diffrn_measurement_device_type  'Rigaku AFC6R'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.02294
_diffrn_reflns_av_sigmaI/netI    0.060
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            11280
_diffrn_reflns_theta_full        59.954
_diffrn_reflns_theta_max         59.954
_diffrn_reflns_theta_min         2.551
_diffrn_standards_decay_%        -6.46
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.876
_exptl_absorpt_correction_T_max  0.555
_exptl_absorpt_correction_T_min  0.392
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
analytical (de Meulenaer & Tompa, 1965)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_density_meas      ?
_exptl_crystal_description       cuboid
_exptl_crystal_F_000             3032
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.07
_refine_diff_density_min         -0.61
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1497
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     856
_refine_ls_number_reflns         8826
_refine_ls_number_restraints     54
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.019
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial,
(Carruthers & Watkin, 1979, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
4.09 -0.747 3.22
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0523
_refine_ls_wR_factor_gt          0.0444
_refine_ls_wR_factor_ref         0.0444
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              25
_reflns_limit_k_min              0
_reflns_limit_l_max              31
_reflns_limit_l_min              0
_reflns_number_gt                8826
_reflns_number_total             10940
_reflns_threshold_expression     I>3.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.95
_oxford_diffrn_Wilson_scale      3.28
_oxford_refine_ls_scale          0.5753(7)
_oxford_structure_analysis_title mat17cu
_cod_data_source_file            b618365d.txt
_cod_data_source_block           benmat17cu
_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 
;
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               7005244