Coordination of Al(C<sub>6</sub>F<sub>5</sub>)<sub>3</sub> <i>vs.</i> B(C<sub>6</sub>F<sub>5</sub>)<sub>3</sub> on group 6 end-on dinitrogen complexes: chemical and structural divergences.
Escomel, Léon; Martins, Frederico F.; Vendier, Laure; Coffinet, Anaïs; Queyriaux, Nicolas; Krewald, Vera; Simonneau, Antoine; Chemical science 15 (2024) 11321–11336; doi:10.1039/d4sc02713b

data_1571917
_publ_section_title
;
 Coordination of Al(C<sub>6</sub>F<sub>5</sub>)<sub>3</sub> <i>vs.</i>
 B(C<sub>6</sub>F<sub>5</sub>)<sub>3</sub> on group 6 end-on dinitrogen
 complexes: chemical and structural divergences.
;
_journal_issue                   29
_journal_name_full               'Chemical science'
_journal_page_first              11321
_journal_page_last               11336
_journal_paper_doi               10.1039/d4sc02713b
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C56 H48 Al2 F30 N4 P4 W, 2(C6 H6)'
_chemical_formula_sum            'C68 H60 Al2 F30 N4 P4 W'
_chemical_formula_weight         1864.88
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_update_record
;
2024-04-09 deposited with the CCDC.	2024-06-16 downloaded from the CCDC.
;
_cell_angle_alpha                92.0780(10)
_cell_angle_beta                 99.059(2)
_cell_angle_gamma                92.5410(10)
_cell_formula_units_Z            4
_cell_length_a                   12.2122(2)
_cell_length_b                   24.4664(3)
_cell_length_c                   25.0551(3)
_cell_measurement_reflns_used    190720
_cell_measurement_temperature    100
_cell_measurement_theta_max      79.15
_cell_measurement_theta_min      2.58
_cell_volume                     7378.43(18)
_computing_cell_refinement
; 
CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)
;
_computing_data_collection       'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_data_reduction
; 
 CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)
;
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.075
_diffrn_reflns_av_unetI/netI     0.052
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            312739
_diffrn_reflns_theta_full        75.593
_diffrn_reflns_theta_max         80.419
_diffrn_reflns_theta_min         2.487
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.044
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.41
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3704
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.020
_refine_diff_density_max         5.95
_refine_diff_density_min         -2.41
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9886
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1963
_refine_ls_number_reflns         31656
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0600
_refine_ls_shift/su_max          0.0013051
_refine_ls_shift/su_mean         0.0000160
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.07P)^2^ +54.68P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1494
_refine_ls_wR_factor_gt          0.1472
_refine_ls_wR_factor_ref         0.1494
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              31
_reflns_limit_k_min              -31
_reflns_limit_l_max              31
_reflns_limit_l_min              0
_reflns_number_gt                29111
_reflns_number_total             31656
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0634
_oxford_refine_ls_scale          0.17781(6)
_oxford_reflns_number_all        31656
_cod_data_source_file            d4sc02713b2.cif
_cod_data_source_block           20230908LeonN
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 1571910--1571919.cif.
;
_cod_original_sg_symbol_Hall     '- P 1'
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               1571917
_oxford_refine_reflns_threshold_expression I>-3.0\s(I)
_oxford_refine_ls_r_factor_all   0.0634
_oxford_refine_ls_wr_factor_all  0.1494