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_4119081
_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;
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_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            'C28 H48 Cl2 Mo2 N12'
_chemical_formula_weight         815.56
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           87
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL--93 and manual editing'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.9752(2)
_cell_length_b                   9.9752(2)
_cell_length_c                   15.8828(2)
_cell_measurement_temperature    150
_cell_volume                     1580.41(5)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150
_diffrn_measurement_device       'Nonius Kappa CCD'
_diffrn_measurement_method       'omega 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  0.0372
_diffrn_reflns_av_sigmaI/netI    0.0162
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19905
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.41
_exptl_absorpt_coefficient_mu    1.005
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.896
_exptl_absorpt_correction_type   Sortav
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_description       chunk
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.137
_refine_ls_goodness_of_fit_obs   1.146
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     72
_refine_ls_number_reflns         942
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.142
_refine_ls_restrained_S_obs      1.151
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_obs          0.0275
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0332P)^2^+3.6035P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0719
_refine_ls_wR_factor_obs         0.0706
_reflns_number_observed          897
_reflns_number_total             942
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja0301065sup1.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0332P)^2^+3.6035P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0332P)^2^+3.6035P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4119081