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_7707304
_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 H66 Al Cu N4 O4, 2(C7 H8)'
_chemical_formula_sum            'C64 H82 Al Cu N4 O4'
_chemical_formula_weight         1061.85
_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     direct
_audit_creation_date             2018-01-16
_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                 97.1641(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1523(2)
_cell_length_b                   27.1205(6)
_cell_length_c                   17.9897(4)
_cell_measurement_reflns_used    4535
_cell_measurement_temperature    173.0(3)
_cell_measurement_theta_max      73.4840
_cell_measurement_theta_min      4.0020
_cell_volume                     5882.7(2)
_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      173.0(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4115
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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      6.00  94.00   1.00   38.92    --   41.86-125.00 -90.00   88
  2  \w     29.00 114.00   1.00   38.92    --   41.86  38.00  60.00   85
  3  \w     38.00 127.00   1.00  155.10    --  106.38 -61.00 -90.00   89
  4  \w     80.00 171.00   1.00  155.10    --  106.38  77.00  30.00   91
  5  \w     36.00  88.00   1.00  155.10    --  106.38 -45.00  90.00   52
  6  \w     92.00 126.00   1.00  155.10    --  106.38 -45.00  90.00   34
  7  \w     49.00 138.00   1.00  155.10    --  106.38 -77.00 120.00   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      -0.0332498000
_diffrn_orient_matrix_UB_12      0.0503208000
_diffrn_orient_matrix_UB_13      -0.0357393000
_diffrn_orient_matrix_UB_21      0.0795097000
_diffrn_orient_matrix_UB_22      -0.0086075000
_diffrn_orient_matrix_UB_23      -0.0591187000
_diffrn_orient_matrix_UB_31      -0.0942801000
_diffrn_orient_matrix_UB_32      -0.0249251000
_diffrn_orient_matrix_UB_33      -0.0517476000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_unetI/netI     0.0814
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18212
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        66.593
_diffrn_reflns_theta_max         66.593
_diffrn_reflns_theta_min         4.012
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.048
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_correction_T_min  0.743
_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    1.199
_exptl_crystal_description       needle
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.633
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.046
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     691
_refine_ls_number_reflns         10285
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1019
_refine_ls_R_factor_gt           0.0573
_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^)+(0.0280P)^2^+4.9460P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1100
_refine_ls_wR_factor_ref         0.1284
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6665
_reflns_number_total             10285
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01415c3.cif
_cod_data_source_block           3h
_cod_depositor_comments
'Adding full bibliography for 7707298--7707305.cif.'
_cod_database_code               7707304
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C64 H82 Al Cu N4 O4'
_chemical_oxdiff_usercomment     RK054
_reflns_odcompleteness_completeness 98.72
_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
C62 \\sim C58 \\sim C63 \\sim C59 \\sim C64 \\sim C60 \\sim C61: within 1.5A
with sigma of 0.04 and sigma for terminal atoms of 0.08
3. Others
 Sof(C159)=Sof(H159)=Sof(C158)=Sof(C163)=Sof(H163)=Sof(C162)=Sof(H162)=
 Sof(C161)=Sof(H161)=Sof(C160)=Sof(H160)=Sof(C164)=Sof(H16A)=Sof(H16B)=
 Sof(H16C)=1-FVAR(1)
 Sof(C58)=Sof(C63)=Sof(H63)=Sof(C62)=Sof(H62)=Sof(C61)=Sof(H61)=Sof(C60)=
 Sof(H60)=Sof(C59)=Sof(H59)=Sof(C64)=Sof(H64A)=Sof(H64B)=Sof(H64C)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C48(H48), C36(H36), C33(H33), C45(H45)
4.b Aromatic/amide H refined with riding coordinates:
 C24(H24), C3(H3), C10(H10), C31(H31), C43(H43), C42(H42), C52(H52), C29(H29),
 C16(H16), C30(H30), C41(H41), C9(H9), C8(H8), C17(H17), C55(H55), C18(H18),
 C53(H53), C54(H54), C56(H56), C63(H63), C62(H62), C61(H61), C60(H60), C59(H59),
  C159(H159), C163(H163), C162(H162), C161(H161), C160(H160)
4.c Fitted hexagon refined as free rotating group:
 C58(C63,C62,C61,C60,C59), C159(C158,C163,C162,C161,C160)
4.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C5(H5A,H5B,H5C), C22(H22A,H22B,H22C), C20(H20A,H20B,
 H20C), C1(H1A,H1B,H1C), C12(H12A,H12B,H12C), C50(H50A,H50B,H50C), C49(H49A,
 H49B,H49C), C38(H38A,H38B,H38C), C13(H13A,H13B,H13C), C34(H34A,H34B,H34C),
 C47(H47A,H47B,H47C), C21(H21A,H21B,H21C), C37(H37A,H37B,H37C), C35(H35A,H35B,
 H35C), C46(H46A,H46B,H46C), C57(H57A,H57B,H57C), C64(H64A,H64B,H64C),
 C164(H16A,H16B,H16C)
;
_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 1.210
_oxdiff_exptl_absorpt_empirical_full_min 0.717