Dinuclear Molybdenum and Tungsten Complexes with Metal-Metal Triple Bonds Supported by p-tert-Butylcalix[4]arene Ligands
Malcolm H. Chisholm; Kirsten Folting; William E. Streib; De-Dong Wu; Inorganic Chemistry 38 (1999) 5219–5229; doi:10.1021/ic990513a

data_5000370
_publ_section_title
;
Dinuclear Molybdenum and Tungsten Complexes with Metal-Metal Triple Bonds
Supported by p-tert-Butylcalix[4]arene Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5219
_journal_page_last               5229
_journal_paper_doi               10.1021/ic990513a
_journal_volume                  38
_journal_year                    1999
_chemical_formula_moiety         '(C88 H104 O8 W2), (H), (C2 H8 N), 7(C6 H6)'
_chemical_formula_sum            'C132 H155 N O8 W2'
_chemical_formula_weight         2251.36
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.421(3)
_cell_length_b                   34.611(3)
_cell_length_c                   13.1126(13)
_cell_measurement_reflns_used    290
_cell_measurement_temperature    106
_cell_measurement_theta_max      11.44
_cell_measurement_theta_min      9.54
_cell_volume                     11537(2)
_diffrn_ambient_temperature      106
_diffrn_detector_area_resol_mean ?
_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  0.063
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            16789
_diffrn_reflns_theta_full        0
_diffrn_reflns_theta_max         25.0873
_diffrn_reflns_theta_min         3.09474
_diffrn_standards_decay_%        -4.9
_diffrn_standards_interval_count 300
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    2.0509
_exptl_absorpt_correction_T_max  0.648
_exptl_absorpt_correction_T_min  0.547
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   Tompa
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'trigonal prism'
_exptl_crystal_F_000             4664
_exptl_crystal_size_max          .30
_exptl_crystal_size_mid          .30
_exptl_crystal_size_min          .25
_refine_diff_density_max         2.7
_refine_diff_density_min         1.0
_refine_ls_abs_structure_details none
_refine_ls_abs_structure_Flack   ?
_refine_ls_extinction_coef       -0.000000015(9)
_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   1.118
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     653
_refine_ls_number_reflns         10300
_refine_ls_R_factor_gt           0.0578
_refine_ls_shift/su_max          0.06
_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         0.0519
_reflns_number_gt                6231
_reflns_number_total             10423
_reflns_threshold_expression     F>3.0\s(F)
_cod_original_formula_sum        'C132 H155 N1 O8 W2'
_cod_database_code               5000370