Nitrogen monoxide and calix[4]pyrrolato aluminate: structural constraint enabled NO dimerization.
Kohl, Senta J.; Sigmund, Lukas M.; Schmitt, Manuel; Greb, Lutz; Chemical science 15 (2024) 10803–10809; doi:10.1039/d4sc02378a

data_1571909
_publ_section_title
;
 Nitrogen monoxide and calix[4]pyrrolato aluminate: structural constraint
 enabled NO dimerization.
;
_journal_issue                   28
_journal_name_full               'Chemical science'
_journal_page_first              10803
_journal_page_last               10809
_journal_paper_doi               10.1039/d4sc02378a
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C34 H37 Al N5 O, C24 H20 P [+ solvent]'
_chemical_formula_sum            'C58 H57 Al N5 O P'
_chemical_formula_weight         898.03
_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     direct
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;FinalCif V130 by Daniel Kratzert, Freiburg 2024, 
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2024-03-21 deposited with the CCDC.	2024-06-17 downloaded from the CCDC.
;
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_cell_angle_beta                 80.317(2)
_cell_angle_gamma                63.381(2)
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_cell_length_b                   13.9223(8)
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_cell_measurement_reflns_used    9380
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.294
_cell_measurement_theta_min      2.6395
_cell_volume                     2667.3(3)
_computing_cell_refinement       'SAINT V8.40B'
_computing_data_collection
'Bruker BIS V6.2.15/2021-03-15 and APEX4 2021.10-0'
_computing_data_reduction        'SAINT V8.40B'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
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_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device       'three-circle diffractometer'
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_diffrn_measurement_method       '\w and \f scans'
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_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            180426
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.812
_diffrn_reflns_theta_min         2.116
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.110
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction: 
Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 
(2015) 3-10
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.118
_exptl_crystal_description       block
_exptl_crystal_F_000             952
_exptl_crystal_recrystallization_method
'Crystallization by vapor diffusion of n-pentane into a DCM/ toluene soltion.'
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.471
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     603
_refine_ls_number_reflns         20863
_refine_ls_number_restraints     1245
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0424
_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^)+(0.0617P)^2^+0.7162P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1122
_refine_ls_wR_factor_ref         0.1225
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16636
_reflns_number_total             20863
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc02378a2.cif
_cod_data_source_block           lms411b_a_sq
_cod_depositor_comments
'Adding full bibliography for 1571908--1571909.cif.'
_cod_database_code               1571909
_shelx_shelxl_version_number     2019/3
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cryostream 800'
_shelx_res_checksum              65947
_shelx_hkl_checksum              96195
_shelx_fab_checksum              92200