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_7707300
_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         'C70 H92 Al2 Co2 N4 O2, 2(C6 H6)'
_chemical_formula_sum            'C82 H104 Al2 Co2 N4 O2'
_chemical_formula_weight         1349.51
_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
_audit_creation_date             2018-11-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-03-17 deposited with the CCDC.	2021-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.8523(19)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.1004(2)
_cell_length_b                   24.5243(3)
_cell_length_c                   12.29286(17)
_cell_measurement_reflns_used    4737
_cell_measurement_temperature    173.00(14)
_cell_measurement_theta_max      72.9720
_cell_measurement_theta_min      4.0510
_cell_volume                     3665.65(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4115
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.952
_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    -25.00  65.00   1.00    5.86    --   42.23 -57.00  90.00   90
  2  \w     34.00 116.00   1.00   24.55    --  105.13-125.00  90.00   82
  3  \w     37.00 131.00   1.00   24.55    --  105.13 -45.00  60.00   94
  4  \w     64.00 165.00   1.00   24.55    --  105.13  15.00  30.00  101
  5  \w     42.00 118.00   1.00   24.55    --  105.13-125.00 -60.00   76
  6  \w     21.00 110.00   1.00    5.86    --   42.23  57.00-120.00   89
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0689297000
_diffrn_orient_matrix_UB_12      -0.0514011000
_diffrn_orient_matrix_UB_13      -0.0041122000
_diffrn_orient_matrix_UB_21      -0.1047442000
_diffrn_orient_matrix_UB_22      0.0352463000
_diffrn_orient_matrix_UB_23      -0.0356344000
_diffrn_orient_matrix_UB_31      -0.0180334000
_diffrn_orient_matrix_UB_32      -0.0080084000
_diffrn_orient_matrix_UB_33      -0.1301419000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12220
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.385
_diffrn_reflns_theta_min         3.605
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.145
_exptl_absorpt_correction_T_max  0.806
_exptl_absorpt_correction_T_min  0.348
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.223
_exptl_crystal_description       needle
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.581
_exptl_crystal_size_mid          0.113
_exptl_crystal_size_min          0.062
_refine_diff_density_max         0.332
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         7023
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0428
_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^)+(0.0408P)^2^+2.0503P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1076
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5595
_reflns_number_total             7023
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01415c3.cif
_cod_data_source_block           3e
_cod_depositor_comments
'Adding full bibliography for 7707298--7707305.cif.'
_cod_original_cell_volume        3665.66(10)
_cod_database_code               7707300
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C82 H104 Al2 Co2 N4 O2'
_chemical_oxdiff_usercomment     RK169
_reflns_odcompleteness_completeness 98.53
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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
C41 \\sim C37 \\sim C36 \\sim C40 \\sim C38 \\sim C39 \\sim C141 \\sim C136
\\sim C140 \\sim C137 \\sim C139 \\sim C138: within 1A with sigma of 0.01 and
sigma for terminal atoms of 0.01
3. Others
 Sof(C136)=Sof(H136)=Sof(C137)=Sof(H137)=Sof(C138)=Sof(H138)=Sof(C139)=
 Sof(H139)=Sof(C140)=Sof(H140)=Sof(C141)=Sof(H141)=1-FVAR(1)
 Sof(C36)=Sof(H36)=Sof(C37)=Sof(H37)=Sof(C38)=Sof(H38)=Sof(C39)=Sof(H39)=
 Sof(C40)=Sof(H40)=Sof(C41)=Sof(H41)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C33(H33), C30(H30), C21(H21), C18(H18)
4.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C9(H9), C14(H14), C26(H26), C4(H4), C2(H2), C27(H27),
 C28(H28), C3(H3), C15(H15), C16(H16), C36(H36), C37(H37), C38(H38), C39(H39),
 C40(H40), C41(H41), C136(H136), C137(H137), C138(H138), C139(H139), C140(H140),
  C141(H141)
4.c Fitted hexagon refined as free rotating group:
 C36(C37,C38,C39,C40,C41), C136(C137,C138,C139,C140,C141)
4.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C22(H22A,H22B,H22C), C35(H35A,H35B,H35C), C20(H20A,H20B,
 H20C), C23(H23A,H23B,H23C), C32(H32A,H32B,H32C), C7(H7A,H7B,H7C), C31(H31A,
 H31B,H31C), C19(H19A,H19B,H19C), C34(H34A,H34B,H34C)
;
_shelx_res_checksum              97854
_shelx_hkl_checksum              36129
_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 1.221
_oxdiff_exptl_absorpt_empirical_full_min 0.621