Synthesis and X-ray Crystal Structure of (tmp)2Al-Fe(cp)(CO)2: An Alanyl-Containing Iron Complex with a Tricoordinated Aluminum Atom
B. N. Anand; Ingo Krossing; Heinrich Nöth; Inorganic Chemistry 36 (1997) 1979–1981; doi:10.1021/ic970110f

data_4323399
_publ_contact_author
;
      Heinrich N\"oth
      Institut f\"ur anorganische Chemie
      Universit\"at M\"unchen
      Meiserstr. 1
      80333 M\"unchen
      Bundesrepublik Deutschland
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_publ_contact_author_email       ui131ac@sunmail.lrz-muenchen.de
_publ_contact_author_fax         '089 5902 451'
_publ_contact_author_phone       '089 5902 396'
_publ_section_title
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 Synthesis and X-ray Crystal Structure of (tmp)2Al-Fe(cp)(CO)2: An
 Alanyl-Containing Iron Complex with a Tricoordinated Aluminum Atom
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1979
_journal_page_last               1981
_journal_paper_doi               10.1021/ic970110f
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C25 H41 Al Fe N2 O2'
_chemical_formula_weight         484.43
_chemical_name_systematic
;
Bis(tetramethylpiperidino)alanyl-cyclopentadienyl-dicarbonyl-iron
;
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-CIF-file updated by CIFRTF'
_cell_angle_alpha                94.015(12)
_cell_angle_beta                 91.184(8)
_cell_angle_gamma                102.496(13)
_cell_formula_units_Z            2
_cell_length_a                   8.347(4)
_cell_length_b                   10.044(5)
_cell_length_c                   15.087(8)
_cell_measurement_reflns_used    152
_cell_measurement_temperature    173
_cell_measurement_theta_max      20.54
_cell_measurement_theta_min      4.36
_cell_volume                     1231.0(11)
_computing_cell_refinement       'SMART (V4.C50)'
_computing_data_collection       'SMART (V4.C50)'
_computing_data_reduction        'SAINT (V4.D50)'
_computing_molecular_graphics    'XP (SHELXTL-Ver.5)'
_computing_publication_material  'SHELXL (Sheldrick 1993'
_computing_structure_refinement  'SHELXL (Sheldrick 1993)'
_computing_structure_solution    'XS (SHELXTL-Ver.5)'
_diffrn_ambient_temperature      173
_diffrn_measurement_device       'Siemens SMART Area-detector'
_diffrn_measurement_method       Hemisphere
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_sigmaI/netI    0.0381
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4819
_diffrn_reflns_theta_max         27.43
_diffrn_reflns_theta_min         1.35
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.672
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_description       needle
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.355
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.179
_refine_ls_goodness_of_fit_obs   1.104
_refine_ls_hydrogen_treatment    'Riding model, fixed isotropic U'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         2967
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.264
_refine_ls_restrained_S_obs      1.104
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_obs          0.0399
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0689P)^2^+2.1826P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1579
_refine_ls_wR_factor_obs         0.1281
_reflns_number_observed          2683
_reflns_number_total             3387
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970110f.cif
_cod_data_source_block           x
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0689P)^2^+2.1826P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0689P)^2^+2.1826P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Heavy atom method' was changed
to 'heavy'.

'_atom_sites_solution_hydrogens' value 'geometrically' was changed to
'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        1231.0(10)
_cod_database_code               4323399