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_7022192
_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         'C38 H53 Al1 Fe1 I1 N3 O2'
_chemical_formula_sum            'C38 H53 Al Fe I N3 O2'
_chemical_formula_weight         793.59
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             11-12-15
_audit_creation_method           CRYSTALS_ver_14.23
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.75650(10)
_cell_length_b                   19.82660(10)
_cell_length_c                   20.35820(10)
_cell_measurement_reflns_used    9362
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     7570.76(7)
_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 0.993
_diffrn_measured_fraction_theta_max 0.992
_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  0.030
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            102060
_diffrn_reflns_theta_full        26.932
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         5.165
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.273
_exptl_absorpt_correction_T_max  0.78
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3280
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.79
_refine_diff_density_min         -0.95
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9418
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         8616
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0325
_refine_ls_shift/su_max          0.0019101
_refine_ls_shift/su_mean         0.0000394
_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:
7.23 10.3 5.05 1.34
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0903
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0902
_reflns_limit_h_max              24
_reflns_limit_h_min              0
_reflns_limit_k_max              25
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                6192
_reflns_number_total             8617
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.94
_oxford_diffrn_Wilson_scale      45.17
_oxford_refine_ls_r_factor_ref   0.0596
_oxford_refine_ls_scale          0.086618(15)
_oxford_reflns_number_all        8617
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 034irnp11
_cod_data_source_file            c2dt31974h.txt
_cod_data_source_block           5
_cod_depositor_comments
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The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
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 b c a '
_cod_original_formula_sum        'C38 H53 Al1 Fe1 I1 N3 O2'
_cod_database_code               7022192
_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 ( 101,X'S)
RIDE C ( 18,X'S) H ( 181,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) H ( 203,X'S) H ( 202,X'S)
RIDE C ( 21,X'S) H ( 211,X'S)
RIDE C ( 22,X'S) H ( 221,X'S)
RIDE C ( 23,X'S) H ( 231,X'S)
RIDE C ( 25,X'S) H ( 251,X'S)
RIDE C ( 26,X'S) H ( 261,X'S) H ( 263,X'S) H ( 262,X'S)
RIDE C ( 27,X'S) H ( 271,X'S) H ( 273,X'S) H ( 272,X'S)
RIDE C ( 29,X'S) H ( 291,X'S)
RIDE C ( 30,X'S) H ( 303,X'S) H ( 302,X'S) H ( 301,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)
RIDE C ( 33,X'S) H ( 333,X'S) H ( 332,X'S) H ( 331,X'S)
RIDE C ( 34,X'S) H ( 343,X'S) H ( 342,X'S) H ( 341,X'S)
RIDE C ( 37,X'S) H ( 371,X'S)
RIDE C ( 38,X'S) H ( 382,X'S) H ( 381,X'S) H ( 383,X'S)
RIDE C ( 39,X'S) H ( 393,X'S) H ( 392,X'S) H ( 391,X'S)
RIDE C ( 40,X'S) H ( 401,X'S)
RIDE C ( 41,X'S) H ( 411,X'S)
RIDE C ( 42,X'S) H ( 421,X'S)
RIDE C ( 44,X'S) H ( 441,X'S)
RIDE C ( 45,X'S) H ( 452,X'S) H ( 451,X'S) H ( 453,X'S)
RIDE C ( 46,X'S) H ( 462,X'S) H ( 461,X'S) H ( 463,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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