Preparation and Characterization of (iPrO)4WW(η2-dmpe)2(CO), (η1-O2CH)(iPrO)4WW(η2-dmpe)2(H), [H(η2-dmpe)WWO2]2(μ-O), and W2(O)4(μ-O)[W(η2-dmpe)2CO]2 (dmpe = Bisdimethylphosphinomethane), Compounds with W-W Bonds between Metal Atoms in Greatly Differing Oxidation States
Malcolm H. Chisholm; Kirsten Folting; Keith S. Kramer; William E. Streib; Inorganic Chemistry 37 (1998) 1549–1554; doi:10.1021/ic9705249

data_4322715
_publ_section_title
;
 Preparation and Characterization of (iPrO)4WW(\h2-dmpe)2(CO),
 (\h1-O2CH)(iPrO)4WW(\h2-dmpe)2(H), [H(\h2-dmpe)WWO2]2(\m-O), and
 W2(O)4(\m-O)[W(\h2-dmpe)2CO]2 (dmpe = Bisdimethylphosphinomethane),
 Compounds with W-W Bonds between Metal Atoms in Greatly Differing
 Oxidation States
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1549
_journal_page_last               1554
_journal_paper_doi               10.1021/ic9705249
_journal_volume                  37
_journal_year                    1998
_chemical_formula_moiety         'C25 H60 O5 P4 W2, 0.5(C7 H8)'
_chemical_formula_sum            'C28.5 H64 O5 P4 W2'
_chemical_formula_weight         978.41
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2bc 2ac'
_symmetry_space_group_name_H-M   'P c a b'
_audit_creation_method
'minor manual editing of SDT2CIF v. 1.1 BETA  output'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.546(3)
_cell_length_b                   21.745(4)
_cell_length_c                   18.114(3)
_cell_measurement_reflns_used    62
_cell_measurement_temperature    102
_cell_measurement_theta_max      15.46
_cell_measurement_theta_min      11.3
_cell_volume                     7699(2)
_computing_cell_refinement       'XTEL, local package'
_computing_data_collection       'NPS, local program'
_computing_data_reduction        'XTEL, local package'
_computing_molecular_graphics    'XTEL, local package'
_computing_publication_material  'XTEL, local package'
_computing_structure_refinement  'XTEL, local package'
_computing_structure_solution    MULTAN78
_diffrn_ambient_temperature      102
_diffrn_measured_fraction_theta_full 0
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device_type  'refurbished Picker diffractometer'
_diffrn_measurement_method       '\q/2\q scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.058
_diffrn_reflns_limit_h_max       +21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       +23
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       +19
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            9921
_diffrn_reflns_theta_full        0
_diffrn_reflns_theta_max         22.5
_diffrn_reflns_theta_min         3.0
_diffrn_standards_decay_%        1.5
_diffrn_standards_interval_count 300
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    6.1764
_exptl_absorpt_correction_T_max  0.608
_exptl_absorpt_correction_T_min  0.252
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   Tompa
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1932
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.41
_refine_diff_density_min         -1.40
_refine_ls_abs_structure_details none
_refine_ls_extinction_coef       0.1357E-7
_refine_ls_extinction_expression
;

Larson, A. C. (1967).  Acta Cryst. 23, p. 664.  Eq. (3)

;
_refine_ls_extinction_method     Zachariasen
_refine_ls_goodness_of_fit_ref   1.1371
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         5056
_refine_ls_R_factor_gt           0.0511
_refine_ls_shift/su_max          0.4859
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w^-1^=\s^2^(F)+(.07F)^2^
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0463
_reflns_number_gt                3940
_reflns_number_total             5056
_reflns_threshold_expression     F>3.0\s(F)
_cod_data_source_file            ic9705249_1.cif
_cod_data_source_block           MSC94102
_cod_database_code               4322715