The syntheses, structures and reactivity of bis(tert-butylcyclopentadienyl)molybdenum derivatives: nitrogen alkylation of an η2-acetonitrile ligand and influence of the chalcogen on the barrier to inversion of chalcogenoether adducts
Shin, Jun Ho; Savage, William; Murphy, Vincent J.; Bonanno, Jeffrey B.; Churchill, David G.; Parkin, Gerard; Journal of the Chemical Society, Dalton Transactions  (2001) 1732–; doi:10.1039/b100372k

data_7010567
_publ_section_title
;
 The syntheses, structures and reactivity of
 bis(tert-butylcyclopentadienyl)molybdenum derivatives: nitrogen
 alkylation of an \h2-acetonitrile ligand and influence of the
 chalcogen on the barrier to inversion of chalcogenoether adducts
;
_journal_issue                   11
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1732
_journal_paper_doi               10.1039/b100372k
_journal_year                    2001
_chemical_formula_sum            'C36 H52 Mo2 Se2'
_chemical_formula_weight         834.58
_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
_cell_angle_alpha                92.13(2)
_cell_angle_beta                 92.25(2)
_cell_angle_gamma                94.92(2)
_cell_formula_units_Z            2
_cell_length_a                   11.023(3)
_cell_length_b                   11.239(3)
_cell_length_c                   14.012(4)
_cell_measurement_reflns_used    42
_cell_measurement_temperature    293(2)
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_cell_measurement_theta_min      5.05
_cell_volume                     1726.7(8)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_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  0.0455
_diffrn_reflns_av_sigmaI/netI    0.1249
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
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_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.82
_diffrn_standards_decay_%        13.18
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.857
_exptl_absorpt_correction_T_max  0.3487
_exptl_absorpt_correction_T_min  0.2048
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Dark_red
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_description       Block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.945
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.134
_refine_ls_extinction_coef       0.0000(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.040
_refine_ls_goodness_of_fit_obs   1.133
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         4446
_refine_ls_number_restraints     136
_refine_ls_restrained_S_all      1.033
_refine_ls_restrained_S_obs      1.116
_refine_ls_R_factor_all          0.1366
_refine_ls_R_factor_obs          0.0678
_refine_ls_shift/esd_max         -2.364
_refine_ls_shift/esd_mean        0.025
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0790P)^2^+0.9507P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1785
_refine_ls_wR_factor_obs         0.1441
_reflns_number_observed          2570
_reflns_number_total             4446
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b100372k.txt
_cod_data_source_block           mose60
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0790P)^2^+0.9507P] 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^)+(0.0790P)^2^+0.9507P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1726.9(8)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7010567