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_7112390
_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_formula_moiety         'C58 H67 Al2 F1 Mo2 N4 O8'
_chemical_formula_sum            'C58 H67 Al2 F Mo2 N4 O8'
_chemical_formula_weight         1213.03
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_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                75.1194(4)
_cell_angle_beta                 88.9465(4)
_cell_angle_gamma                85.7380(4)
_cell_formula_units_Z            2
_cell_length_a                   9.80680(10)
_cell_length_b                   17.0565(2)
_cell_length_c                   18.6455(2)
_cell_measurement_reflns_used    12963
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     3005.89(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 0.991
_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  0.026
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            100852
_diffrn_reflns_theta_full        26.938
_diffrn_reflns_theta_max         27.488
_diffrn_reflns_theta_min         5.122
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.503
_exptl_absorpt_correction_T_max  0.94
_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            yellow
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1252
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.130
_refine_diff_density_max         1.08
_refine_diff_density_min         -0.88
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9335
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     763
_refine_ls_number_reflns         13693
_refine_ls_number_restraints     256
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0415
_refine_ls_shift/su_max          0.0094287
_refine_ls_shift/su_mean         0.0003675
_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:
16.0 23.0 11.0 2.84
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1098
_refine_ls_wR_factor_gt          0.0917
_refine_ls_wR_factor_ref         0.1098
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              22
_reflns_limit_k_min              -21
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                10735
_reflns_number_total             13693
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.38
_oxford_diffrn_Wilson_scale      13.96
_oxford_refine_ls_r_factor_ref   0.0592
_oxford_refine_ls_scale          0.27859(14)
_oxford_reflns_number_all        13693
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title '005rtrt12 At 23: 7 on 28/ 8'
_cod_data_source_file            c3cc42342e.txt
_cod_data_source_block           1
_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 -1 '
_cod_original_formula_sum        'C58 H67 Al2 F1 Mo2 N4 O8'
_cod_database_code               7112390
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S
CONT H ( 1,X'S,U[ISO]) H ( 4,X'S,U[ISO]) H ( 6,X'S,U[ISO])
CONT H ( 3,X'S,U[ISO]) H ( 5,X'S,U[ISO]) H ( 7,X'S,U[ISO])
REM RIDE MO ( 1,X'S) H ( 1,X'S) H ( 4,X'S)
REM RIDE AL ( 2,X'S) H ( 1,X'S) H ( 4,X'S) H ( 6,X'S)
RIDE C ( 5,X'S) H ( 51,X'S) H ( 52,X'S)
RIDE C ( 6,X'S) H ( 61,X'S) H ( 62,X'S)
RIDE C ( 7,X'S) H ( 71,X'S) H ( 72,X'S)
RIDE C ( 11,X'S) H ( 111,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)
RIDE C ( 16,X'S) H ( 161,X'S) H ( 162,X'S) H ( 163,X'S)
RIDE C ( 17,X'S) H ( 171,X'S) H ( 172,X'S) H ( 173,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 ( 241,X'S) H ( 242,X'S) H ( 243,X'S)
RIDE C ( 25,X'S) H ( 251,X'S) H ( 252,X'S) H ( 253,X'S)
RIDE C ( 26,X'S) H ( 263,X'S) H ( 262,X'S) H ( 261,X'S)
REM RIDE MO ( 35,X'S) H ( 3,X'S) H ( 5,X'S)
REM RIDE AL ( 36,X'S) H ( 3,X'S) H ( 5,X'S) H ( 7,X'S)
RIDE C ( 41,X'S) H ( 411,X'S) H ( 412,X'S) H ( 413,X'S)
RIDE C ( 42,X'S) H ( 421,X'S)
RIDE C ( 44,X'S) H ( 441,X'S) H ( 442,X'S) H ( 443,X'S)
RIDE C ( 45,X'S) H ( 451,X'S)
RIDE C ( 47,X'S) H ( 471,X'S) H ( 472,X'S) H ( 473,X'S)
RIDE C ( 48,X'S) H ( 481,X'S) H ( 482,X'S)
RIDE C ( 49,X'S) H ( 491,X'S) H ( 492,X'S)
RIDE C ( 50,X'S) H ( 501,X'S) H ( 502,X'S)
RIDE C ( 54,X'S) H ( 541,X'S) H ( 542,X'S) H ( 543,X'S)
RIDE C ( 55,X'S) H ( 551,X'S)
RIDE C ( 57,X'S) H ( 571,X'S) H ( 572,X'S) H ( 573,X'S)
RIDE C ( 58,X'S) H ( 581,X'S)
RIDE C ( 60,X'S) H ( 601,X'S) H ( 602,X'S) H ( 603,X'S)
RIDE C ( 73,X'S) H ( 731,X'S)
RIDE C ( 74,X'S) H ( 741,X'S)
RIDE C ( 75,X'S) H ( 751,X'S)
RIDE C ( 76,X'S) H ( 761,X'S)
RIDE C ( 77,X'S) H ( 771,X'S)
RIDE C ( 78,X'S) H ( 781,X'S)
RIDE C ( 79,X'S) H ( 791,X'S)
RIDE C ( 80,X'S) H ( 801,X'S)
RIDE C ( 81,X'S) H ( 811,X'S)
RIDE C ( 82,X'S) H ( 821,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
SAME F(69) C(71) C(73) C(76) C(78) C(79) C(81) AND
CONT F(69) C(71) C(81) C(79) C(78) C(76) C(73) AND
CONT F(70) C(72) C(74) C(75) C(77) C(80) C(82) AND
CONT F(70) C(72) C(82) C(80) C(77) C(75) C(74)
SIMU 0.01 F(69) C(71) C(73) C(76) C(78) C(79) C(81) AND
CONT F(69) C(71) C(81) C(79) C(78) C(76) C(73) AND
CONT F(70) C(72) C(74) C(75) C(77) C(80) C(82) AND
CONT F(70) C(72) C(82) C(80) C(77) C(75) C(74)
DELU 0.01 F(69) C(71) C(73) C(76) C(78) C(79) C(81) AND
CONT F(69) C(71) C(81) C(79) C(78) C(76) C(73) AND
CONT F(70) C(72) C(74) C(75) C(77) C(80) C(82) AND
CONT F(70) C(72) C(82) C(80) C(77) C(75) C(74)
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;