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_7707305
_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         'C46 H54 Al Cl4 Cu N4'
_chemical_formula_sum            'C46 H54 Al Cl4 Cu N4'
_chemical_formula_weight         895.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-02-09
_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                 96.1813(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.11938(13)
_cell_length_b                   20.2656(2)
_cell_length_c                   20.5958(2)
_cell_measurement_reflns_used    5435
_cell_measurement_temperature    173.00(14)
_cell_measurement_theta_max      73.5860
_cell_measurement_theta_min      4.3040
_cell_volume                     4614.09(8)
_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    'olex2.solve (Bourhis et al., 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 0.955
_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      3.00  92.00   1.00    9.63    --   41.98-125.00  60.00   89
  2  \w    -11.00  70.00   1.00    9.63    --   41.98 -57.00 150.00   81
  3  \w     35.00 121.00   1.00   60.96    --  106.38-125.00 -60.00   86
  4  \w     79.00 170.00   1.00   60.96    --  106.38  61.00-180.00   91
  5  \w     39.00 129.00   1.00   60.96    --  106.38 -61.00  30.00   90
  6  \w     81.00 168.00   1.00   60.96    --  106.38 125.00  60.00   87
;
_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      0.1144451000
_diffrn_orient_matrix_UB_12      -0.0403174000
_diffrn_orient_matrix_UB_13      0.0224177000
_diffrn_orient_matrix_UB_21      0.0175597000
_diffrn_orient_matrix_UB_22      0.0402564000
_diffrn_orient_matrix_UB_23      0.0638285000
_diffrn_orient_matrix_UB_31      -0.0774408000
_diffrn_orient_matrix_UB_32      -0.0503443000
_diffrn_orient_matrix_UB_33      0.0329814000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_av_unetI/netI     0.0778
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15323
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.851
_diffrn_reflns_theta_min         4.318
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.252
_exptl_absorpt_correction_T_max  0.890
_exptl_absorpt_correction_T_min  0.662
_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    1.289
_exptl_crystal_description       needle
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.198
_exptl_crystal_size_mid          0.069
_exptl_crystal_size_min          0.044
_refine_diff_density_max         0.402
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         8930
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0443
_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^)+(0.0446P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1177
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6828
_reflns_number_total             8930
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01415c3.cif
_cod_data_source_block           3g
_cod_depositor_comments
'Adding full bibliography for 7707298--7707305.cif.'
_cod_original_cell_volume        4614.09(9)
_cod_database_code               7707305
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C46 H54 Al Cl4 Cu N4'
_chemical_oxdiff_usercomment     RK052
_reflns_odcompleteness_completeness 98.79
_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.a Ternary CH refined with riding coordinates:
 C29(H29), C41(H41), C44(H44), C32(H32)
2.b Aromatic/amide H refined with riding coordinates:
 C25(H25), C9(H9), C20(H20), C26(H26), C3(H3), C15(H15), C16(H16), C27(H27),
 C39(H39), C10(H10), C8(H8), C38(H38), C37(H37), C14(H14)
2.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C1(H1A,H1B,H1C), C22(H22A,H22B,H22C), C33(H33A,H33B,H33C),
 C31(H31A,H31B,H31C), C30(H30A,H30B,H30C), C42(H42A,H42B,H42C), C43(H43A,H43B,
 H43C), C46(H46A,H46B,H46C), C34(H34A,H34B,H34C), C18(H18A,H18B,H18C), C45(H45A,
 H45B,H45C)
;
_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 1.280
_oxdiff_exptl_absorpt_empirical_full_min 0.503