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_4322716
_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         'C26 H64 O7 P8 W4, 4(C H2 Cl2)'
_chemical_formula_sum            'C30 H72 Cl8 O7 P8 W4'
_chemical_formula_weight         1811.67
_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'
_audit_creation_method
'minor manual editing of SDT2CIF v. 1.1 BETA  output'
_cell_angle_alpha                90
_cell_angle_beta                 97.880(11)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.282(2)
_cell_length_b                   14.308(3)
_cell_length_c                   15.319(3)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    104
_cell_measurement_theta_max      16.96
_cell_measurement_theta_min      12.56
_cell_volume                     2883.7(9)
_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      104
_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  0.029
_diffrn_reflns_limit_h_max       +14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       +12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7225
_diffrn_reflns_theta_full        0
_diffrn_reflns_theta_max         22.5
_diffrn_reflns_theta_min         3.0
_diffrn_standards_decay_%        1.2
_diffrn_standards_interval_count 300
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    8.5898
_exptl_absorpt_correction_T_max  0.516
_exptl_absorpt_correction_T_min  0.256
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   Tompa
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.086
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelopiped
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.6
_refine_diff_density_min         -0.7
_refine_ls_abs_structure_details none
_refine_ls_extinction_coef       0.3431E-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   0.8656
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         3775
_refine_ls_R_factor_gt           0.0245
_refine_ls_shift/su_max          0.17
_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         0.0266
_reflns_number_gt                3414
_reflns_number_total             3775
_reflns_threshold_expression     F>3.0\s(F)
_cod_data_source_file            ic9705249_2.cif
_cod_data_source_block           MSC94233
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4322716