Syntheses, Structures, and Reactivities of 2,3-Pyrazyl-Linked Bis(1-aza-allyl) Alkali-Metal Complexes
Leung, Wing-Por; Ip, Queenie Wai-Yan; Lam, Tai-Wing; Mak, Thomas C. W.; Organometallics 23 (2004) 1284–; doi:10.1021/om034323q

data_4076275
_publ_section_title
;
 Syntheses, Structures, and Reactivities of 2,3-Pyrazyl-Linked
 Bis(1-aza-allyl) Alkali-Metal Complexes
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1284
_journal_paper_doi               10.1021/om034323q
_journal_volume                  23
_journal_year                    2004
_chemical_formula_sum            'C29 H59 Mg N3 O P2 Si2'
_chemical_formula_weight         608.22
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.0880(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   38.2658(18)
_cell_length_b                   10.8370(5)
_cell_length_c                   18.0881(9)
_cell_measurement_temperature    293(2)
_cell_volume                     7275.3(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0395
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            24044
_diffrn_reflns_theta_full        28.04
_diffrn_reflns_theta_max         28.04
_diffrn_reflns_theta_min         1.10
_exptl_absorpt_coefficient_mu    0.227
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.771105
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_density_diffrn    1.111
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2656
_exptl_crystal_size_max          1.20
_exptl_crystal_size_mid          0.62
_exptl_crystal_size_min          0.41
_refine_diff_density_max         0.482
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         8785
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0853
_refine_ls_R_factor_gt           0.0548
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1102P)^2^+0.3691P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1509
_refine_ls_wR_factor_ref         0.1775
_reflns_number_gt                5867
_reflns_number_total             8785
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om034323qsi20031125_104155.cif
_cod_data_source_block           Mg
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'MONOCLINIC' changed to 'monoclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4076275