Synthesis, Structure, and Density Functional Theory Analysis of a Scandium Dinitrogen Complex, [(C5Me4H)2Sc]2(μ-η2:η2-N2)
Selvan Demir; Sara E. Lorenz; Ming Fang; Filipp Furche; Gerd Meyer; Joseph W. Ziller; William J. Evans; Journal of the American Chemical Society 132 (2010) 11151–11158; doi:10.1021/ja102681w

data_4102824
_publ_contact_author
; 
Professor William J. Evans
Department of Chemistry
1102 Natural Sciences II
University of California, Irvine
Irvine, CA 92697-2025
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_publ_contact_author_email       wevans@uci.edu
_publ_contact_author_fax         '1  949 824 2210'
_publ_contact_author_phone       '1  949 824 5174'
_publ_section_title
;
 Synthesis, Structure, and Density Functional Theory Analysis of a
 Scandium Dinitrogen Complex, [(C5Me4H)2Sc]2(\m-\h2:\h2-N2)
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_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11151
_journal_page_last               11158
_journal_paper_doi               10.1021/ja102681w
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C72 H104 N2 O Sc4'
_chemical_formula_weight         1193.41
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 91.485(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.8370(14)
_cell_length_b                   21.042(3)
_cell_length_c                   17.909(3)
_cell_measurement_reflns_used    5661
_cell_measurement_temperature    148(2)
_cell_measurement_theta_max      20.95
_cell_measurement_theta_min      2.25
_cell_volume                     3329.0(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      148(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \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  0.1026
_diffrn_reflns_av_sigmaI/netI    0.1312
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27208
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    0.433
_exptl_absorpt_correction_T_max  0.9720
_exptl_absorpt_correction_T_min  0.9281
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            gold
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1284
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.737
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     744
_refine_ls_number_reflns         9526
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1125
_refine_ls_R_factor_gt           0.0675
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0772P)^2^+0.3286P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1437
_refine_ls_wR_factor_ref         0.1647
_reflns_number_gt                6548
_reflns_number_total             9526
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja102681w_si_006.cif
_cod_data_source_block           sd26
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        3329.1(9)
_cod_database_code               4102824