Salt metathesis for the synthesis of M-Al and M-H-Al bonds.
Riddlestone, Ian M.; Urbano, Juan; Phillips, Nicholas; Kelly, Michael J.; Vidovic, Dragoslav; Bates, Joshua I.; Taylor, Russell; Aldridge, Simon; Dalton transactions (Cambridge, England : 2003) 42 (2013) 249–258; doi:10.1039/c2dt31974h

data_7022191
_publ_section_title
;
 Salt metathesis for the synthesis of M-Al and M-H-Al bonds.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              249
_journal_page_last               258
_journal_paper_doi               10.1039/c2dt31974h
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C31 H51 Al1 Cl1 Fe1 N3 O2'
_chemical_formula_sum            'C31 H51 Al Cl Fe N3 O2'
_chemical_formula_weight         616.05
_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     direct
_audit_creation_date             12-08-01
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                89.0196(18)
_cell_angle_beta                 71.366(2)
_cell_angle_gamma                80.7037(15)
_cell_formula_units_Z            2
_cell_length_a                   10.5121(4)
_cell_length_b                   11.4183(4)
_cell_length_c                   14.4923(6)
_cell_measurement_reflns_used    6381
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     1625.57(11)
_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 0.979
_diffrn_measured_fraction_theta_max 0.974
_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  0.020
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21942
_diffrn_reflns_theta_full        25.548
_diffrn_reflns_theta_max         27.471
_diffrn_reflns_theta_min         5.159
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.604
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             660.000
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.85
_refine_diff_density_min         -0.63
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9257
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         7264
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.0018998
_refine_ls_shift/su_mean         0.0000648
_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:
116. 188. 114. 47.3 10.9
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1243
_refine_ls_wR_factor_gt          0.1083
_refine_ls_wR_factor_ref         0.1242
_reflns_limit_h_max              13
_reflns_limit_h_min              -12
_reflns_limit_k_max              14
_reflns_limit_k_min              -14
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                5801
_reflns_number_total             7265
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.90
_oxford_diffrn_Wilson_scale      0.98
_oxford_refine_ls_r_factor_ref   0.0621
_oxford_refine_ls_scale          1.019(3)
_oxford_reflns_number_all        7265
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title '020irnp11 At 16:51 on 29/ 6'
_cod_data_source_file            c2dt31974h.txt
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C31 H51 Al1 Cl1 Fe1 N3 O2'
_cod_database_code               7022191
_iucr_refine_instruction_details_constraints
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BLOCK SCALE X'S, U'S
RIDE C(14,U'S) C(114,U'S)
RIDE C(15,U'S) C(115,U'S)
EQUIV PART(1001,OCC) PART(1002,OCC)
WEIGHT -1 PART(1002,OCC)
RIDE C ( 7,X'S) H ( 71,X'S)
RIDE C ( 8,X'S) H ( 82,X'S) H ( 81,X'S)
RIDE C ( 9,X'S) H ( 91,X'S) H ( 92,X'S)
RIDE C ( 10,X'S) H ( 101,X'S) H ( 102,X'S)
RIDE C ( 11,X'S) H ( 111,X'S) H ( 112,X'S)
RIDE C ( 12,X'S) H ( 121,X'S) H ( 122,X'S)
RIDE C ( 14,X'S) H ( 141,X'S)
RIDE C ( 15,X'S) H ( 152,X'S) H ( 151,X'S) H ( 153,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)
RIDE C ( 18,X'S) H ( 182,X'S) H ( 181,X'S) H ( 183,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 ( 21,X'S) H ( 212,X'S) H ( 211,X'S)
RIDE C ( 22,X'S) H ( 221,X'S) H ( 222,X'S)
RIDE C ( 23,X'S) H ( 232,X'S) H ( 231,X'S)
RIDE C ( 24,X'S) H ( 241,X'S) H ( 242,X'S)
RIDE C ( 25,X'S) H ( 251,X'S) H ( 252,X'S)
RIDE C ( 31,X'S) H ( 311,X'S) H ( 313,X'S) H ( 312,X'S)
RIDE C ( 32,X'S) H ( 321,X'S) H ( 323,X'S) H ( 322,X'S)
RIDE C ( 33,X'S) H ( 331,X'S) H ( 332,X'S) H ( 333,X'S)
RIDE C ( 34,X'S) H ( 341,X'S) H ( 342,X'S) H ( 343,X'S)
RIDE C ( 35,X'S) H ( 351,X'S) H ( 352,X'S) H ( 353,X'S)
RIDE C ( 114,X'S) H (1141,X'S)
RIDE C ( 115,X'S) H (1152,X'S) H (1151,X'S) H (1153,X'S)
RIDE C ( 116,X'S) H (1162,X'S) H (1161,X'S) H (1163,X'S)
END
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_iucr_refine_instruction_details_restraints
;
SAME N(13) C(14) C(15) C(16) AND
CONT N(13) C(14) C(16) C(15) AND
CONT N(13) C(114) C(115) C(116) AND
CONT N(13) C(114) C(116) C(115)
REM DELU START (DO NOT REMOVE THIS LINE)
VIBR .0, 0.00200 = C(14) TO C(16)
VIBR .0, 0.00500 = C(16) TO N(13)
VIBR .0, 0.00500 = C(16) TO C(15)
VIBR .0, 0.00200 = C(114) TO C(116)
VIBR .0, 0.00500 = C(116) TO N(13)
VIBR .0, 0.00500 = C(116) TO C(115)
REM DELU END (DO NOT REMOVE THIS LINE)
REM THERMSIM START (DO NOT REMOVE THIS LINE)
U(IJ) .0, 0.08000 = C(14) TO C(16)
U(IJ) .0, 0.08000 = C(114) TO C(116)
REM THERMSIM END (DO NOT REMOVE THIS LINE)
END
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