σ-Alane Complexes of Chromium, Tungsten, and Manganese
Ian M. Riddlestone; Siân Edmonds; Paul A. Kaufman; Juan Urbano Baena; Joshua I. Bates; Michael J. Kelly; Amber L. Thompson; Russell Taylor; Simon Aldridge; Journal of the American Chemical Society 134 (2012) 2551–2554; doi:10.1021/ja2119892

data_4117444
_publ_contact_author             'Simon Aldridge'
_publ_contact_author_email       Simon.aldridge@chem.ox.ac.uk
_publ_section_title
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 \s-Alane Complexes of Chromium, Tungsten, and Manganese
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_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2551
_journal_page_last               2554
_journal_paper_doi               10.1021/ja2119892
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C36 H50 Al1 N3 O5 W1'
_chemical_formula_sum            'C36 H50 Al N3 O5 W'
_chemical_formula_weight         815.64
_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   difmap
_atom_sites_solution_primary     other
_audit_creation_date             11-12-05
_audit_creation_method           CRYSTALS_ver_14.23
_cell_angle_alpha                90
_cell_angle_beta                 98.4228(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.64322(10)
_cell_length_b                   19.59951(19)
_cell_length_c                   18.60077(18)
_cell_measurement_reflns_used    13637
_cell_measurement_temperature    150
_cell_measurement_theta_max      76.3953
_cell_measurement_theta_min      3.2917
_cell_volume                     3838.31(6)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'Xcalibur, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction XCALIBUR'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22161
_diffrn_reflns_theta_full        74.289
_diffrn_reflns_theta_max         76.587
_diffrn_reflns_theta_min         3.294
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.131
_exptl_absorpt_correction_T_max  0.54
_exptl_absorpt_correction_T_min  0.43
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_description       block
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.01
_refine_diff_density_min         -1.09
_refine_ls_extinction_coef       39.7(8)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.4791
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         7964
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0286
_refine_ls_R_factor_gt           0.0272
_refine_ls_shift/su_max          0.0019908
_refine_ls_shift/su_mean         0.0000341
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 551. 686. 243. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0420
_refine_ls_wR_factor_gt          0.0418
_refine_ls_wR_factor_ref         0.0420
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              24
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                7543
_reflns_number_total             7994
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.93
_oxford_diffrn_Wilson_scale      0.15
_oxford_refine_ls_r_factor_ref   0.0286
_oxford_refine_ls_scale          2.794(10)
_oxford_reflns_number_all        7964
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 0632irmk11
_cod_data_source_file            ja2119892_si_002_4.cif
_cod_data_source_block           3
_cod_original_cell_volume        3838.30(6)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C36 H50 Al1 N3 O5 W1'
_cod_database_code               4117444
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S, H(21,X'S), H(22,X'S) 
CONT EXTPARAM 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) H   ( 132,X'S) H   ( 133,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) H   ( 142,X'S) H   ( 143,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) H   ( 163,X'S) H   ( 162,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) H   ( 173,X'S) H   ( 172,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  20,X'S) H   ( 202,X'S) H   ( 201,X'S) H   ( 203,X'S) 
RIDE C   (  21,X'S) H   ( 212,X'S) H   ( 211,X'S) H   ( 213,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 232,X'S) H   ( 231,X'S) H   ( 233,X'S) 
RIDE C   (  24,X'S) H   ( 242,X'S) H   ( 241,X'S) H   ( 243,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) H   ( 282,X'S) H   ( 283,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) H   ( 292,X'S) H   ( 293,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) H   ( 353,X'S) H   ( 352,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) H   ( 363,X'S) H   ( 362,X'S) 
END                                                                             
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_iucr_refine_instruction_details_restraints
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REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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