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_4119083
_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 N12 W2'
_chemical_formula_weight         1713.63
_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     heavy
_audit_creation_method           'SHELXL-93 plus editing'
_cell_angle_alpha                75.728(1)
_cell_angle_beta                 81.398(1)
_cell_angle_gamma                85.268(1)
_cell_formula_units_Z            1
_cell_length_a                   10.3837(1)
_cell_length_b                   11.1668(1)
_cell_length_c                   13.3458(1)
_cell_measurement_reflns_used    88608
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.26
_cell_volume                     1481.17(2)
_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  0.0561
_diffrn_reflns_av_sigmaI/netI    0.0328
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            48929
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    4.822
_exptl_absorpt_correction_T_max  0.627
_exptl_absorpt_correction_T_min  0.500
_exptl_absorpt_correction_type   Sortav
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.921
_exptl_crystal_description       chunk
_exptl_crystal_F_000             830
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.203
_refine_diff_density_min         -0.905
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.035
_refine_ls_goodness_of_fit_obs   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         6792
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_restrained_S_obs      1.055
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_obs          0.0250
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0267P)^2^+1.6164P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0575
_refine_ls_wR_factor_obs         0.0554
_reflns_number_observed          6117
_reflns_number_total             6792
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja0301065sup3.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^)+(0.0267P)^2^+1.6164P] 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^)+(0.0267P)^2^+1.6164P] 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               4119083