Poly(pyrazolyl)aluminate Complexes Containing Aluminum-Hydrogen Bonds
Christopher J. Snyder; Mary Jane Heeg; Charles H. Winter; Inorganic Chemistry 50 (2011) 9210–9212; doi:10.1021/ic201541c

data_4326421
_publ_contact_author             'Prof. Charles H. Winter'
_publ_contact_author_address
; Department of Chemistry
     Wayne State University
 Detroit, Michigan 48202
 USA
;
_publ_contact_author_email       chw@chem.wayne.edu
_publ_section_title
;
 Poly(pyrazolyl)aluminate Complexes Containing Aluminum-Hydrogen Bonds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9210
_journal_page_last               9212
_journal_paper_doi               10.1021/ic201541c
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C49 H42 Al Li N6 O'
_chemical_formula_weight         764.81
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.9991(6)
_cell_length_b                   17.6024(5)
_cell_length_c                   22.6480(6)
_cell_measurement_reflns_used    8076
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.1
_cell_measurement_theta_min      2.7
_cell_volume                     7972.8(4)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker APEX2'
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_method       'Bruker APEX2'
_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  0.0977
_diffrn_reflns_av_sigmaI/netI    0.0864
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            203899
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         33.12
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    0.097
_exptl_absorpt_correction_T_max  0.9874
_exptl_absorpt_correction_T_min  0.9520
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick, 1997'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_description       'cut fragment'
_exptl_crystal_F_000             3216
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     527
_refine_ls_number_reflns         14684
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1180
_refine_ls_R_factor_gt           0.0543
_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^)+(0.0532P)^2^+1.4140P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1065
_refine_ls_wR_factor_ref         0.1248
_reflns_number_gt                8817
_reflns_number_total             14684
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201541c_si_002_3.cif
_cod_data_source_block           hder
_cod_database_code               4326421