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_7707303
_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         'C50 H74 Al Fe N2 O3 P, C7 H8'
_chemical_formula_sum            'C57 H82 Al Fe N2 O3 P'
_chemical_formula_weight         957.04
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-03-20
_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                 102.825(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0053(4)
_cell_length_b                   16.6674(5)
_cell_length_c                   23.4517(10)
_cell_measurement_reflns_used    4701
_cell_measurement_temperature    173.05(10)
_cell_measurement_theta_max      27.4830
_cell_measurement_theta_min      2.9790
_cell_volume                     5337.8(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      173.05(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0382
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.807
_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    -13.00  74.00   1.00   24.91    --   14.27  19.00 150.00   87
  2  \w     -5.00  80.00   1.00   24.91    --   14.27  37.00-150.00   85
;
_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      0.0403022000
_diffrn_orient_matrix_UB_12      -0.0165198000
_diffrn_orient_matrix_UB_13      0.0203769000
_diffrn_orient_matrix_UB_21      -0.0326937000
_diffrn_orient_matrix_UB_22      -0.0176570000
_diffrn_orient_matrix_UB_23      0.0155266000
_diffrn_orient_matrix_UB_31      -0.0025584000
_diffrn_orient_matrix_UB_32      -0.0349992000
_diffrn_orient_matrix_UB_33      -0.0174966000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0624
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.807
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            19253
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.807
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.307
_diffrn_reflns_theta_min         2.565
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.373
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.893
_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    1.191
_exptl_crystal_description       prism
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.564
_exptl_crystal_size_mid          0.176
_exptl_crystal_size_min          0.139
_refine_diff_density_max         0.585
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     659
_refine_ls_number_reflns         10728
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0923
_refine_ls_R_factor_gt           0.0598
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0757P)^2^+3.0702P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1425
_refine_ls_wR_factor_ref         0.1649
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7543
_reflns_number_total             10728
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01415c3.cif
_cod_data_source_block           3d
_cod_depositor_comments
'Adding full bibliography for 7707298--7707305.cif.'
_cod_database_code               7707303
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C50 H74 Al Fe N2 O3 P'
_reflns_odcompleteness_completeness 98.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C39 \\sim C40 \\sim C43 \\sim C44 \\sim C42 \\sim C41 \\sim C143 \\sim C144
\\sim C140 \\sim C141 \\sim C142: within 1.4A with sigma of 0.01 and sigma for
terminal atoms of 0.01
C55 \\sim C54 \\sim C56 \\sim C155 \\sim C156 \\sim C53 \\sim C52 \\sim C51
\\sim C57 \\sim C154 \\sim C151 \\sim C152 \\sim C153 \\sim C157: within 1A
with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C57) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(C154)=Sof(H154)=Sof(C155)=Sof(H155)=Sof(C156)=Sof(H156)=Sof(C151)=
 Sof(C152)=Sof(H152)=Sof(C153)=Sof(H153)=Sof(C157)=Sof(H15A)=Sof(H15B)=
 Sof(H15C)=1-FVAR(1)
 Sof(C55)=Sof(H55)=Sof(C54)=Sof(H54)=Sof(C53)=Sof(H53)=Sof(C52)=Sof(H52)=
 Sof(C51)=Sof(C56)=Sof(H56)=Sof(C57)=Sof(H57A)=Sof(H57B)=Sof(H57C)=FVAR(1)
 Sof(H39A)=Sof(C143)=Sof(H14A)=Sof(H14B)=Sof(C144)=Sof(H14C)=Sof(H14D)=
 Sof(C140)=Sof(H14E)=Sof(H14F)=Sof(C141)=Sof(H14G)=Sof(H14H)=Sof(C142)=
 Sof(H14I)=Sof(H14J)=1-FVAR(2)
 Sof(H39)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(C44)=
 Sof(H44A)=Sof(H44B)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(C41)=Sof(H41A)=Sof(H41B)=
 FVAR(2)
4.a Ternary CH refined with riding coordinates:
 C18(H18), C15(H15), C30(H30), C27(H27), C45(H45), C33(H33), C39(H39), C39(H39A)
4.b Secondary CH2 refined with riding coordinates:
 C50(H50A,H50B), C49(H49A,H49B), C40(H40A,H40B), C46(H46A,H46B), C48(H48A,
 H48B), C36(H36A,H36B), C43(H43A,H43B), C47(H47A,H47B), C44(H44A,H44B),
 C42(H42A,H42B), C41(H41A,H41B), C38(H38A,H38B), C34(H34A,H34B), C37(H37A,H37B),
  C35(H35A,H35B), C143(H14A,H14B), C144(H14C,H14D), C140(H14E,H14F), C141(H14G,
 H14H), C142(H14I,H14J)
4.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C6(H6), C25(H25), C23(H23), C13(H13), C12(H12), C24(H24), C55(H55),
 C54(H54), C53(H53), C52(H52), C56(H56), C154(H154), C155(H155), C156(H156),
 C152(H152), C153(H153)
4.d Fitted hexagon refined as free rotating group:
 C55(C54,C53,C52,C51,C56), C154(C155,C156,C151,C152,C153)
4.e Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C4(H4A,H4B,H4C), C32(H32A,H32B,H32C), C17(H17A,H17B,H17C),
 C19(H19A,H19B,H19C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C16(H16A,H16B,
 H16C), C20(H20A,H20B,H20C), C31(H31A,H31B,H31C), C57(H57A,H57B,H57C),
 C157(H15A,H15B,H15C)
;
_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 1.197
_oxdiff_exptl_absorpt_empirical_full_min 0.788