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_7022189
_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         'C20 H33 Al1 Cl1 Fe1 N3 O2'
_chemical_formula_sum            'C20 H33 Al Cl Fe N3 O2'
_chemical_formula_weight         465.78
_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             12-03-26
_audit_creation_method           CRYSTALS_ver_14.11
_cell_angle_alpha                92.0036(7)
_cell_angle_beta                 92.5025(7)
_cell_angle_gamma                100.7188(6)
_cell_formula_units_Z            4
_cell_length_a                   8.72890(10)
_cell_length_b                   15.4840(2)
_cell_length_c                   17.7812(3)
_cell_measurement_reflns_used    9687
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     2356.82(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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.984
_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  0.053
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            34511
_diffrn_reflns_theta_full        26.193
_diffrn_reflns_theta_max         27.571
_diffrn_reflns_theta_min         5.108
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.810
_exptl_absorpt_correction_T_max  0.86
_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    1.313
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_refine_diff_density_max         1.05
_refine_diff_density_min         -0.65
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9869
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         10737
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0924
_refine_ls_R_factor_gt           0.0724
_refine_ls_shift/su_max          0.0004435
_refine_ls_shift/su_mean         0.0000175
_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:
35.0 54.9 31.7 12.4 2.72
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2072
_refine_ls_wR_factor_gt          0.1886
_refine_ls_wR_factor_ref         0.2072
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              20
_reflns_limit_k_min              -20
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                8511
_reflns_number_total             10737
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.06
_oxford_diffrn_Wilson_scale      11.02
_oxford_refine_ls_r_factor_ref   0.0924
_oxford_refine_ls_scale          0.3182(5)
_oxford_reflns_number_all        10737
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title '7110911 Compound X'
_cod_data_source_file            c2dt31974h.txt
_cod_data_source_block           2b
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C20 H33 Al1 Cl1 Fe1 N3 O2'
_cod_database_code               7022189
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S
SUMFIX ELEMENT SCALES
END
;
_iucr_refine_instruction_details_restraints
;
NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;