Calix[4]pyrrolato gallate: square planar-coordinated gallium(iii) and its metal–ligand cooperative reactivity with CO2 and alcohols
Sigmund, Lukas M.; Engels, Eliane; Richert, Nick; Greb, Lutz; Chemical Science 13 (2022) 11215–11220; doi:10.1039/D2SC03054C

data_1567603
_publ_section_title
;
 Calix[4]pyrrolato gallate: square planar-coordinated gallium(iii) and its
 metal--ligand cooperative reactivity with CO2 and alcohols
;
_journal_issue                   37
_journal_name_full               'Chemical Science'
_journal_page_first              11215
_journal_page_last               11220
_journal_paper_doi               10.1039/D2SC03054C
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         'C32 H40 Ga N4 O, C24 H20 P'
_chemical_formula_sum            'C56 H60 Ga N4 O P'
_chemical_formula_weight         905.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method
;
FinalCif V104 by Daniel Kratzert, Freiburg 2022,
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2022-05-31 deposited with the CCDC.	2022-09-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.630(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_c                   17.1423(7)
_cell_measurement_reflns_used    9248
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5385
_cell_measurement_theta_min      2.5155
_cell_volume                     4543.9(4)
_computing_cell_refinement       'SAINT V8.40B'
_computing_data_reduction        'SAINT V8.40B'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
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_diffrn_detector_type            'Bruker PHOTON III'
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_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE dual wavelength Mo/Cu'
_diffrn_measurement_method       '\w and \f scans'
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_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
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_diffrn_reflns_limit_l_min       -22
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_diffrn_reflns_point_group_measured_fraction_full 0.998
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_diffrn_source                   'microfocus sealed X-ray tube'
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_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
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_exptl_absorpt_correction_T_min  0.6661
_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    1.324
_exptl_crystal_description       block
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          0.694
_exptl_crystal_size_mid          0.453
_exptl_crystal_size_min          0.342
_refine_diff_density_max         0.432
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     576
_refine_ls_number_reflns         10488
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0358P)^2^+1.8378P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0689
_refine_ls_wR_factor_ref         0.0700
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9810
_reflns_number_total             10488
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc03054c2.cif
_cod_data_source_block           mo_LMSEE019_0m
_cod_depositor_comments
'Adding full bibliography for 1567601--1567603.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1567603
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.647
_shelx_estimated_absorpt_t_max   0.799
_olex2_diffrn_ambient_temperature_device 'Oxford Cryostream 800'
_shelx_res_checksum              49781
_shelx_hkl_checksum              89089