1<sup>st</sup> row transition metal aluminylene complexes: preparation, properties and bonding analysis.
Kong, Richard Y.; Crimmin, Mark R.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 7810–7817; doi:10.1039/d1dt01415c

data_7707302
_publ_section_title
;
 1<sup>st</sup> row transition metal aluminylene complexes: preparation,
 properties and bonding analysis.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7810
_journal_page_last               7817
_journal_paper_doi               10.1039/d1dt01415c
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C33 H41 Al Fe N2 O4, C7 H8'
_chemical_formula_sum            'C40 H49 Al Fe N2 O4'
_chemical_formula_weight         704.64
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-03-07
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2021-03-17 deposited with the CCDC.	2021-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.9278(9)
_cell_length_b                   16.6105(8)
_cell_length_c                   10.6008(6)
_cell_measurement_reflns_used    1948
_cell_measurement_temperature    173.00(14)
_cell_measurement_theta_max      26.8840
_cell_measurement_theta_min      2.9200
_cell_volume                     3861.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0382
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.820
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -10.00  16.00   1.00  220.68    --  -13.18 -99.00 120.00   26
  2  \w     -1.00  81.00   1.00  220.68    --   14.27  57.00-120.00   82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0320276000
_diffrn_orient_matrix_UB_12      0.0049004000
_diffrn_orient_matrix_UB_13      0.0055024000
_diffrn_orient_matrix_UB_21      -0.0012671000
_diffrn_orient_matrix_UB_22      -0.0147785000
_diffrn_orient_matrix_UB_23      0.0627246000
_diffrn_orient_matrix_UB_31      0.0043539000
_diffrn_orient_matrix_UB_32      -0.0397678000
_diffrn_orient_matrix_UB_33      -0.0226123000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.820
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            8626
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.820
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.334
_diffrn_reflns_theta_min         2.279
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.454
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.912
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_description       plate
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.339
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.027
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         4086
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0450
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0687P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1310
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2941
_reflns_number_total             4086
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01415c3.cif
_cod_data_source_block           3c
_cod_depositor_comments
'Adding full bibliography for 7707298--7707305.cif.'
_cod_original_cell_volume        3861.2(3)
_cod_database_code               7707302
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C33 H41 Al Fe N2 O4'
_chemical_oxdiff_usercomment     RK077
_reflns_odcompleteness_completeness 98.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C19 \\sim C25 \\sim C122
\\sim C123 \\sim C124 \\sim C119 \\sim C120 \\sim C121 \\sim C125: within 1A
with sigma of 0.02 and sigma for terminal atoms of 0.02
3. Others
 Sof(C122)=Sof(H122)=Sof(C123)=Sof(H123)=Sof(C124)=Sof(H124)=Sof(C119)=
 Sof(C120)=Sof(H120)=Sof(C121)=Sof(H121)=Sof(C125)=Sof(H12A)=Sof(H12B)=
 Sof(H12C)=0.5*(1-FVAR(2))
 Sof(C20)=Sof(H20)=Sof(C21)=Sof(H21)=Sof(C22)=Sof(H22)=Sof(C23)=Sof(H23)=
 Sof(C24)=Sof(H24)=Sof(C19)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=0.5*FVAR(2)
4.a Ternary CH refined with riding coordinates:
 C13(H13), C16(H16)
4.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C11(H11), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C23(H23),
 C24(H24), C122(H122), C123(H123), C124(H124), C120(H120), C121(H121)
4.c Fitted hexagon refined as free rotating group:
 C20(C21,C22,C23,C24,C19), C122(C123,C124,C119,C120,C121)
4.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C15(H15C,H15B,
 H15A), C14(H14C,H14A,H14B), C25(H25A,H25B,H25C), C125(H12A,H12B,H12C)
;
_ins_header
;
TITL MRC1823 in Pnma 
REM Pnma (#62, found as Pcmn in -cba setting)
CELL 0.71073  21.927777  16.610512  10.600843  90.0000  90.0000  90.0000
ZERR    4.00   0.000941   0.000781   0.000565   0.0000   0.0000   0.0000
LATT  1
SYMM -x+1/2,-y, z+1/2 
SYMM -x, y+1/2,-z 
SYMM  x+1/2,-y+1/2,-z+1/2 
SFAC C H N O Al Fe
UNIT 132.00 164.00 8.00 16.00 4.00 4.00
TREF
HKLF 4
END
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.036
_oxdiff_exptl_absorpt_empirical_full_min 0.976