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_7022187
_publ_section_title
;
 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         'C13 H19 Al1 Cl2 N2'
_chemical_formula_sum            'C13 H19 Al Cl2 N2'
_chemical_formula_weight         301.19
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             11-12-05
_audit_creation_method           CRYSTALS_ver_14.11
_cell_angle_alpha                90
_cell_angle_beta                 113.5072(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4052(3)
_cell_length_b                   11.0555(2)
_cell_length_c                   11.9482(2)
_cell_measurement_reflns_used    1894
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     1623.78(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 0.990
_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  0.011
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10036
_diffrn_reflns_theta_full        26.942
_diffrn_reflns_theta_max         27.492
_diffrn_reflns_theta_min         5.219
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.440
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_correction_T_min  0.56
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.740
_exptl_crystal_size_mid          0.380
_exptl_crystal_size_min          0.360
_refine_diff_density_max         0.32
_refine_diff_density_min         -0.32
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8663
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     86
_refine_ls_number_reflns         1845
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0312
_refine_ls_shift/su_max          0.0002415
_refine_ls_shift/su_mean         0.0000273
_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:
93.6 153. 91.4 37.9 9.14
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0884
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0884
_reflns_limit_h_max              15
_reflns_limit_h_min              -17
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                1683
_reflns_number_total             1845
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.74
_oxford_diffrn_Wilson_scale      0.62
_oxford_refine_ls_r_factor_ref   0.0349
_oxford_refine_ls_scale          1.044(5)
_oxford_reflns_number_all        1845
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title '12051505 004juct10'
_cod_data_source_file            c2dt31974h.txt
_cod_data_source_block           1c
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_original_formula_sum        'C13 H19 Al1 Cl2 N2'
_cod_database_code               7022187
_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 ( 71,X'S)
RIDE C ( 8,X'S) H ( 81,X'S)
RIDE C ( 9,X'S) H ( 91,X'S)
RIDE C ( 10,X'S) H ( 103,X'S) H ( 102,X'S) H ( 101,X'S)
RIDE C ( 11,X'S) H ( 113,X'S) H ( 112,X'S) H ( 111,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
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