Reversible OH-Bond Activation and Amphoterism by Metal-Ligand Cooperativity of the Calix[4]pyrrolato Aluminate
Sigmund, Lukas M.; Greb, Lutz; Chemical Science  (2020) –; doi:10.1039/D0SC03602A

data_1558886
_publ_section_title
;
 Reversible OH-Bond Activation and Amphoterism by Metal-Ligand
 Cooperativity of the Calix[4]pyrrolato Aluminate
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC03602A
_journal_year                    2020
_chemical_formula_moiety         'C34 H37 Al Br N4 O, C24 H20 P, 2(C H2 Cl2)'
_chemical_formula_sum            'C60 H61 Al Br Cl4 N4 O P'
_chemical_formula_weight         1133.78
_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     dual
_audit_creation_date             2020-05-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-06-30 deposited with the CCDC.	2020-08-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.380(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7658(18)
_cell_length_b                   27.696(6)
_cell_length_c                   20.719(4)
_cell_measurement_reflns_used    9071
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      29.33
_cell_measurement_theta_min      2.26
_cell_volume                     5473.6(19)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0993
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            227575
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         2.013
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.037
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6080
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1400 before and 0.0857 after correction.
The Ratio of minimum to maximum transmission is 0.8150.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_description       block
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          0.258
_exptl_crystal_size_mid          0.246
_exptl_crystal_size_min          0.132
_refine_diff_density_max         0.988
_refine_diff_density_min         -0.842
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     657
_refine_ls_number_reflns         10164
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0472
_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^)+(0.0732P)^2^+7.7741P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1251
_refine_ls_wR_factor_ref         0.1338
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8858
_reflns_number_total             10164
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc03602a2.cif
_cod_data_source_block           mo_lms44b_ii_0ma
_cod_database_code               1558886
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.875
_shelx_estimated_absorpt_t_min   0.776
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1)
2.b Secondary CH2 refined with riding coordinates:
 C301(H30A,H30B), C201(H20A,H20B)
2.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C30(H30), C31(H31), C17(H17), C18(H18), C122(H122), C123(H123),
 C12(H12), C106(H106), C124(H124), C102(H102), C121(H121), C7(H7), C3(H3),
 C105(H105), C120(H120), C8(H8), C34(H34), C33(H33), C2(H2), C117(H117),
 C116(H116), C118(H118), C110(H110), C108(H108), C114(H114), C112(H112),
 C109(H109), C115(H115), C103(H103), C104(H104), C111(H111)
2.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C25(H25A,H25B,H25C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C28(H28A,H28B,H28C), C22(H22A,H22B,H22C), C21(H21A,
 H21B,H21C)
;
_shelx_res_checksum              59910
_olex2_submission_special_instructions 'No special instructions were received'