Sodium Polypyrazolylaluminates: Synthesis, Characterization, and Isolation of a Reaction Intermediate of a Trispyrazolylaluminate
Cortes-Llamas, Sara A.; Muñoz-Hernández, Miguel-Ángel; Organometallics 26 (2007) 6844–; doi:10.1021/om700828b

data_4074026
_publ_section_title
;
 Sodium Polypyrazolylaluminates: Synthesis, Characterization, and
 Isolation of a Reaction Intermediate of a Trispyrazolylaluminate
;
_journal_issue                   27
_journal_name_full               Organometallics
_journal_page_first              6844
_journal_paper_doi               10.1021/om700828b
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C77 H136 Al2 N12 Na2'
_chemical_formula_weight         618.49
_chemical_name_common            'Compound 4'
_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-97
_cell_angle_alpha                95.412(2)
_cell_angle_beta                 99.459(2)
_cell_angle_gamma                110.421(2)
_cell_formula_units_Z            2
_cell_length_a                   9.8013(13)
_cell_length_b                   10.5746(14)
_cell_length_c                   21.951(3)
_cell_measurement_temperature    100(2)
_cell_volume                     2074.6(5)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0278
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            20218
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.034
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             698
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.193
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         7299
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          6.884
_refine_ls_shift/su_mean         0.017
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0746P)^2^+0.6450P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1274
_refine_ls_wR_factor_ref         0.1313
_reflns_number_gt                6563
_reflns_number_total             7299
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700828b-file004.cif
_cod_data_source_block           sara8m
_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C77 H136 N12 Na2 Al2'
_cod_database_code               4074026