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_7707301
_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         'C52 H64 Al Cu F6 N4'
_chemical_formula_sum            'C52 H64 Al Cu F6 N4'
_chemical_formula_weight         949.58
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-11-13
_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                88.586(3)
_cell_angle_beta                 88.722(3)
_cell_angle_gamma                67.821(4)
_cell_formula_units_Z            2
_cell_length_a                   11.1165(4)
_cell_length_b                   12.5995(5)
_cell_length_c                   19.3405(8)
_cell_measurement_reflns_used    4678
_cell_measurement_temperature    173.00(14)
_cell_measurement_theta_max      28.1050
_cell_measurement_theta_min      2.7820
_cell_volume                     2507.43(18)
_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 16.0382
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.798
_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    -40.00  52.00   1.00   35.48    --  -13.18  77.00  90.00   92
  2  \w    -78.00  11.00   1.00   35.48    --  -13.18 -77.00 -30.00   89
  3  \w     -2.00  82.00   1.00   35.48    --   14.27  57.00-120.00   84
;
_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      -0.0646331000
_diffrn_orient_matrix_UB_12      0.0074316000
_diffrn_orient_matrix_UB_13      0.0095276000
_diffrn_orient_matrix_UB_21      0.0235565000
_diffrn_orient_matrix_UB_22      -0.0387368000
_diffrn_orient_matrix_UB_23      0.0283016000
_diffrn_orient_matrix_UB_31      -0.0040525000
_diffrn_orient_matrix_UB_32      0.0462742000
_diffrn_orient_matrix_UB_33      0.0213151000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0182
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.798
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14639
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.798
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.268
_diffrn_reflns_theta_min         2.229
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.513
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97224
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_description       plate
_exptl_crystal_F_000             1000
_exptl_crystal_preparation       'Recrystallisation from toluene'
_exptl_crystal_size_max          0.414
_exptl_crystal_size_mid          0.178
_exptl_crystal_size_min          0.086
_refine_diff_density_max         0.319
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     593
_refine_ls_number_reflns         9920
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0412
_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^)+(0.0567P)^2^+0.4441P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.1149
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7902
_reflns_number_total             9920
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01415c3.cif
_cod_data_source_block           3f
_cod_depositor_comments
;
Adding full bibliography for 7707298--7707305.cif.

2025-03-06
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         474.79
_cod_original_formula_moiety         '0.5(C52 H64 Al Cu F6 N4)'
_cod_original_formula_units_Z            4
_cod_original_formula_sum        'C26 H32 Al0.50 Cu0.50 F3 N2'
_cod_database_code               7707301
_shelx_shelxl_version_number     2016/6
_publ_section_exptl
;
Any special experimental details
;
_chemical_oxdiff_formula         'C52 H64 Al Cu F6 N4'
_chemical_oxdiff_usercomment     RK020
_reflns_odcompleteness_completeness 98.98
_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.a Ternary CH refined with riding coordinates:
 C38(H38), C50(H50), C48(H48), C35(H35)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C10(H10), C17(H17), C31(H31), C26(H26), C19(H19), C33(H33), C44(H44),
 C45(H45), C8(H8), C43(H43), C32(H32)
2.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C28(H28A,H28B,H28C), C21(H21A,H21B,H21C), C40(H40A,H40B,
 H40C), C13(H13A,H13B,H13C), C12(H12A,H12B,H12C), C51(H51A,H51B,H51C), C14(H14A,
 H14B,H14C), C49(H49A,H49B,H49C), C47(H47A,H47B,H47C), C22(H22A,H22B,H22C),
 C52(H52A,H52B,H52C), C39(H39A,H39B,H39C), C36(H36A,H36B,H36C), C23(H23C,H23A,
 H23B), C37(H37A,H37B,H37C)
;
_shelx_res_checksum              57466
_shelx_hkl_checksum              99453
_ins_header
;
TITL MRC1783_red in P-1 
REM P-1 (#2 in standard setting)
CELL 0.71073  11.116515  12.599540  19.340494  88.5859  88.7216  67.8205
ZERR    2.00   0.000392   0.000522   0.000811   0.0034   0.0032   0.0036
LATT  1
SFAC C H N F Al Cu
UNIT 104.00 128.00 8.00 12.00 2.00 2.00
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 1.049
_oxdiff_exptl_absorpt_empirical_full_min 0.954