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_5000371
_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 Mo2 O8), 2(C2 H8 N), 4(C5 H5 N)'
_chemical_formula_sum            'C112 H140 Mo2 N6 O8'
_chemical_formula_weight         1890.26
_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'
_cell_angle_alpha                90
_cell_angle_beta                 100.264(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.3843(17)
_cell_length_b                   22.130(3)
_cell_length_c                   18.621(3)
_cell_measurement_reflns_used    164
_cell_measurement_temperature    105
_cell_measurement_theta_max      17.4
_cell_measurement_theta_min      11.9
_cell_volume                     5021.7(13)
_diffrn_ambient_temperature      105
_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  0.039
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10086
_diffrn_reflns_theta_full        0
_diffrn_reflns_theta_max         22.5375
_diffrn_reflns_theta_min         3.13085
_diffrn_standards_decay_%        -0.8
_diffrn_standards_interval_count 300
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    0.3083
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            amber
_exptl_crystal_density_diffrn    1.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2004
_exptl_crystal_size_max          .25
_exptl_crystal_size_mid          .25
_exptl_crystal_size_min          .08
_refine_diff_density_max         1.6
_refine_diff_density_min         -0.70
_refine_ls_abs_structure_details none
_refine_ls_abs_structure_Flack   ?
_refine_ls_extinction_coef       -0.00000019(4)
_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   1.2484
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         6577
_refine_ls_R_factor_gt           0.0585
_refine_ls_shift/su_max          0.167
_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         0.0584
_reflns_number_gt                4799
_reflns_number_total             6577
_reflns_threshold_expression     F>3.0\s(F)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               5000371