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_7022194
_publ_section_title
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 Salt metathesis for the synthesis of M-Al and M-H-Al bonds.
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_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         'C27 H44 Al1 Fe1 N3 O2'
_chemical_formula_sum            'C27 H44 Al Fe N3 O2'
_chemical_formula_weight         525.49
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             11-10-24
_audit_creation_method           CRYSTALS_ver_14.11
_cell_angle_alpha                81.6863(7)
_cell_angle_beta                 83.7688(7)
_cell_angle_gamma                82.6593(7)
_cell_formula_units_Z            2
_cell_length_a                   9.91410(10)
_cell_length_b                   11.3263(2)
_cell_length_c                   12.8550(2)
_cell_measurement_reflns_used    6160
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     1410.63(4)
_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 0.991
_diffrn_measured_fraction_theta_max 0.990
_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  0.057
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            25106
_diffrn_reflns_theta_full        25.549
_diffrn_reflns_theta_max         27.473
_diffrn_reflns_theta_min         5.187
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.593
_exptl_absorpt_correction_T_max  0.95
_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            colourless
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             564
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.91
_refine_diff_density_min         -0.83
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9102
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         6408
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0959
_refine_ls_R_factor_gt           0.0480
_refine_ls_shift/su_max          0.0001105
_refine_ls_shift/su_mean         0.0000078
_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:
3.73 4.06 0.980
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1478
_refine_ls_wR_factor_gt          0.0937
_refine_ls_wR_factor_ref         0.1478
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              14
_reflns_limit_k_min              -14
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                3965
_reflns_number_total             6408
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.03
_oxford_diffrn_Wilson_scale      19.43
_oxford_refine_ls_r_factor_ref   0.0959
_oxford_refine_ls_scale          0.22771(17)
_oxford_reflns_number_all        6408
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title '10241000 Compound X'
_cod_data_source_file            c2dt31974h.txt
_cod_data_source_block           7
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C27 H44 Al1 Fe1 N3 O2'
_cod_database_code               7022194
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S
RIDE C ( 6,X'S) H ( 61,X'S)
RIDE C ( 7,X'S) H ( 72,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 ( 13,X'S) H ( 131,X'S)
RIDE C ( 14,X'S) H ( 142,X'S) H ( 143,X'S) H ( 141,X'S)
RIDE C ( 15,X'S) H ( 151,X'S) H ( 153,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 ( 172,X'S) H ( 173,X'S)
RIDE C ( 18,X'S) H ( 182,X'S) H ( 183,X'S) H ( 181,X'S)
RIDE C ( 19,X'S) H ( 191,X'S)
RIDE C ( 20,X'S) H ( 202,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 ( 231,X'S) H ( 232,X'S)
RIDE C ( 24,X'S) H ( 241,X'S) H ( 242,X'S)
RIDE C ( 25,X'S) H ( 29,X'S)
RIDE C ( 28,X'S) H ( 281,X'S)
RIDE C ( 29,X'S) H ( 291,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)
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)
END
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