Al-H σ-bond coordination: expanded ring carbene adducts of AlH3 as neutral bi- and tri-functional donor ligands.
Abdalla, Joseph A. B.; Riddlestone, Ian M.; Tirfoin, Remi; Phillips, Nicholas; Bates, Joshua I.; Aldridge, Simon; Chemical communications (Cambridge, England) 49 (2013) 5547–5549; doi:10.1039/c3cc42342e

data_7112388
_publ_section_title
;
 Al-H \s-bond coordination: expanded ring carbene adducts of AlH3 as
 neutral bi- and tri-functional donor ligands.
;
_journal_issue                   49
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5547
_journal_page_last               5549
_journal_paper_doi               10.1039/c3cc42342e
_journal_volume                  49
_journal_year                    2013
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C22 H31 Al1 N2'
_chemical_formula_sum            'C22 H31 Al N2'
_chemical_formula_weight         350.48
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P -2n -2ac'
_symmetry_space_group_name_H-M   'P c 21 n'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             13-03-25
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.10950(10)
_cell_length_b                   15.6301(3)
_cell_length_c                   16.3634(3)
_cell_measurement_reflns_used    2595
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     2074.10(6)
_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    'Superflip (Palatinus & Chapuis, 2007)'
_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  0.025
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23363
_diffrn_reflns_theta_full        26.664
_diffrn_reflns_theta_max         27.488
_diffrn_reflns_theta_min         5.152
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.104
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.122
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.310
_exptl_crystal_size_min          0.210
_refine_diff_density_max         0.27
_refine_diff_density_min         -0.29
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9516
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         2447
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          0.0004174
_refine_ls_shift/su_mean         0.0000311
_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:
43.2 71.9 44.9 19.6 4.87
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1008
_refine_ls_wR_factor_gt          0.0889
_refine_ls_wR_factor_ref         0.1008
_reflns_limit_h_max              10
_reflns_limit_h_min              0
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                2140
_reflns_number_total             2447
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.38
_oxford_diffrn_Wilson_scale      3.34
_oxford_refine_ls_r_factor_ref   0.0507
_oxford_refine_ls_scale          0.5293(14)
_oxford_reflns_number_all        2447
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_oxford_structure_analysis_title '020jart13 At 23:14 on 13/ 1'
_cod_data_source_file            c3cc42342e.txt
_cod_data_source_block           020jart13
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      'P c 21 n '
_cod_original_formula_sum        'C22 H31 Al1 N2'
_cod_database_code               7112388
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S
CONT H ( 1,X'S,U[ISO]) H(2,X'S,U[ISO]) H (5,X'S,U[ISO])
REM RIDE AL ( 1,X'S) H ( 1,X'S) H ( 2,X'S) H ( 5,X'S)
RIDE C ( 6,X'S) H ( 61,X'S) H ( 63,X'S) H ( 62,X'S)
RIDE C ( 7,X'S) H ( 71,X'S)
RIDE C ( 9,X'S) H ( 91,X'S)
RIDE C ( 11,X'S) H ( 111,X'S) H ( 112,X'S) H ( 113,X'S)
RIDE C ( 12,X'S) H ( 122,X'S) H ( 121,X'S) H ( 123,X'S)
RIDE C ( 13,X'S) H ( 132,X'S) H ( 131,X'S)
RIDE C ( 14,X'S) H ( 141,X'S) H ( 142,X'S)
RIDE C ( 15,X'S) H ( 152,X'S) H ( 151,X'S)
RIDE C ( 19,X'S) H ( 191,X'S) H ( 193,X'S) H ( 192,X'S)
RIDE C ( 20,X'S) H ( 201,X'S)
RIDE C ( 22,X'S) H ( 221,X'S)
RIDE C ( 24,X'S) H ( 242,X'S) H ( 241,X'S) H ( 243,X'S)
RIDE C ( 25,X'S) H ( 252,X'S) H ( 251,X'S) H ( 253,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;