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_4326419
_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            'C46 H54 Cl2 Co2 N4 O4'
_chemical_formula_weight         915.69
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 99.310(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.1641(10)
_cell_length_b                   12.7107(11)
_cell_length_c                   30.885(3)
_cell_measurement_reflns_used    2940
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      18.8
_cell_measurement_theta_min      2.5
_cell_volume                     4325.0(7)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.203
_diffrn_reflns_av_sigmaI/netI    0.1923
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            75662
_diffrn_reflns_theta_full        28.26
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         1.34
_exptl_absorpt_coefficient_mu    0.938
_exptl_absorpt_correction_T_max  0.8674
_exptl_absorpt_correction_T_min  0.6491
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick, 1997'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_description       rod
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.840
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         10687
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.2062
_refine_ls_R_factor_gt           0.0770
_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^)+(0.0678P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1416
_refine_ls_wR_factor_ref         0.1882
_reflns_number_gt                4617
_reflns_number_total             10687
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201541c_si_002_1.cif
_cod_data_source_block           arit
_cod_database_code               4326419