M2(hpp)4Cl2and M2(hpp)4, Where M = Mo and W: Preparations, Structure and Bonding, and Comparisons with C2, C2H2, and C2Cl2and the Hypothetical Molecules M2(hpp)4(H)2†
Chisholm, Malcolm H.; Gallucci, Judith; Hadad, Christopher M.; Huffman, John C.; Wilson, Paul J.; Journal of the American Chemical Society 125 (2003) 16040–16049; doi:10.1021/ja0301065

data_4119082
_publ_section_title
;
 M2(hpp)4Cl2and M2(hpp)4, Where M = Mo and W:&#x00A0; Preparations,
 Structure and Bonding, and Comparisons with C2, C2H2, and C2Cl2and the
 Hypothetical Molecules M2(hpp)4(H)2&#x2020;
;
_journal_issue                   51
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16040
_journal_page_last               16049
_journal_paper_doi               10.1021/ja0301065
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C34 H48 Cl20 D6 Mo2 N12'
_chemical_formula_weight         1537.84
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                75.7020(10)
_cell_angle_beta                 81.7050(10)
_cell_angle_gamma                85.3730(10)
_cell_formula_units_Z            1
_cell_length_a                   10.3116(4)
_cell_length_b                   11.1805(4)
_cell_length_c                   13.2926(5)
_cell_measurement_reflns_used    4314
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      25.4
_cell_measurement_theta_min      2.7
_cell_volume                     1467.86(10)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999), XTEL (local package)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 44.52
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
'   0.30 degree frames measured for  30.16 seconds each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0847
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8498
_diffrn_reflns_theta_full        30.02
_diffrn_reflns_theta_max         30.02
_diffrn_reflns_theta_min         2.39
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    1.378
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'thin plate'
_exptl_crystal_density_diffrn    1.740
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       brown/green
_exptl_crystal_F_000             766
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.679
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.772
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         8498
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.772
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0347
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc 
 [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/ 
   [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0000P)^2^+0.0000sin\q/\l] 
 where P = 1.00000Fo^2^ + 0.00000Fc^2^ 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0576
_refine_ls_wR_factor_ref         0.0629
_reflns_number_gt                5976
_reflns_number_total             8498
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0301065sup2.cif
_cod_data_source_block           d:\99077\99077
_cod_database_code               4119082