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_4117445
_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
'0.89(C33 H43 Al1 Cr1 N2 O4), 0.11(C34 H43 Al1 Cr1 N2 O5)'
_chemical_formula_sum            'C33.11 H43 Al Cr N2 O4.11'
_chemical_formula_weight         613.89
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             11-12-02
_audit_creation_method           CRYSTALS_ver_14.30
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.5944(2)
_cell_length_b                   21.1678(3)
_cell_length_c                   9.0757(1)
_cell_measurement_reflns_used    4319
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     3380.11(7)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.019
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7354
_diffrn_reflns_theta_full        27.473
_diffrn_reflns_theta_max         27.473
_diffrn_reflns_theta_min         5.146
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.401
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.96
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_description       block
_exptl_crystal_F_000             1303.0
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.66
_refine_diff_density_min         -0.58
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9421
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         3950
_refine_ls_number_restraints     360
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0456
_refine_ls_shift/su_max          0.0005214
_refine_ls_shift/su_mean         0.0000416
_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: 
 54.7 90.8 54.9 22.7 4.97 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1103
_refine_ls_wR_factor_gt          0.1025
_refine_ls_wR_factor_ref         0.1103
_reflns_limit_h_max              22
_reflns_limit_h_min              0
_reflns_limit_k_max              0
_reflns_limit_k_min              -27
_reflns_limit_l_max              0
_reflns_limit_l_min              -11
_reflns_number_gt                3280
_reflns_number_total             3951
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.29
_oxford_diffrn_Wilson_scale      8.67
_oxford_refine_ls_r_factor_ref   0.0569
_oxford_refine_ls_scale          0.3856(6)
_oxford_reflns_number_all        3951
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 014pkir11
_cod_data_source_file            ja2119892_si_002_5.cif
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      'P n m a '
_cod_original_formula_sum        'C33.11 H43 Al1 Cr1 N2 O4.11'
_cod_database_code               4117445
_iucr_refine_instruction_details_constraints
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BLOCK SCALE X'S 
CONT FIRST(U'S) UNTIL CR(101) 
CONT AL(102,U[ISO]) UNTIL O(126) 
EQUIV PART(1001,OCC) PART(1002,OCC) 
WEIGHT -1 PART(1002,OCC) 
RIDE CR  (   1,X'S) H   (  11,X'S) H   (  12,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   6,X'S) H   (  63,X'S) H   (  61,X'S) H   (  62,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 142,X'S) H   ( 141,X'S) H   ( 143,X'S) 
RIDE C   (  15,X'S) H   ( 153,X'S) H   ( 151,X'S) H   ( 152,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) H   ( 173,X'S) H   ( 172,X'S) 
RIDE C   (  18,X'S) H   ( 182,X'S) H   ( 181,X'S) H   ( 183,X'S) 
RIDE CR  ( 101,X'S) H   (1011,X'S) 
RIDE AL  ( 102,X'S) H   (1012,X'S) 
END                                                                             
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_iucr_refine_instruction_details_restraints
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NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
REM   SHIFTLIMIT   START (DO NOT REMOVE THIS LINE) 
LIMIT      0.01000000 U[ISO] 
LIMIT      0.01000000 X 
LIMIT      0.01000000 y
LIMIT      0.01000000 Z 
LIMIT      0.01000000 U[11] 
LIMIT      0.01000000 U[22] 
LIMIT      0.01000000 U[33] 
LIMIT      0.01000000 U[12] 
LIMIT      0.01000000 U[13] 
LIMIT      0.01000000 U[23] 
LIMIT      0.01000000 OCC 
REM   SHIFTLIMIT   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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