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_1567602
_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         'C28 H32 Ga N4, C24 H20 P, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C52.5 H53 Cl Ga N4 P'
_chemical_formula_weight         876.13
_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     dual
_audit_creation_date             2020-10-08
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2022-05-31 deposited with the CCDC.	2022-09-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.797(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.4110(18)
_cell_length_b                   16.6359(13)
_cell_length_c                   23.7139(18)
_cell_measurement_reflns_used    9782
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.44
_cell_measurement_theta_min      2.18
_cell_volume                     9545.0(13)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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  0.0912
_diffrn_reflns_av_unetI/netI     0.0553
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            141733
_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         26.999
_diffrn_reflns_theta_min         2.054
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.704
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6782
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1674 before and 0.0751 after correction.
The Ratio of minimum to maximum transmission is 0.9094.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_description       block
_exptl_crystal_F_000             3672
_exptl_crystal_size_max          0.144
_exptl_crystal_size_mid          0.113
_exptl_crystal_size_min          0.086
_refine_diff_density_max         1.470
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1088
_refine_ls_number_reflns         20825
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0517P)^2^+6.3639P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1083
_refine_ls_wR_factor_ref         0.1219
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14897
_reflns_number_total             20825
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc03054c2.cif
_cod_data_source_block           mo_lmsnr006_ii_02a
_cod_depositor_comments
'Adding full bibliography for 1567601--1567603.cif.'
_cod_original_cell_volume        9545.0(12)
_cod_original_formula_sum        'C52.50 H53 Cl Ga N4 P'
_cod_database_code               1567602
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.942
_shelx_estimated_absorpt_t_min   0.905
_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 Secondary CH2 refined with riding coordinates:
 C401(H40A,H40B)
2.b Aromatic/amide H refined with riding coordinates:
 C218(H218), C224(H224), C220(H220), C314(H314), C215(H215), C320(H320),
 C8(H8), C221(H221), C12(H12), C223(H223), C318(H318), C302(H302), C7(H7),
 C3(H3), C214(H214), C222(H222), C206(H206), C13(H13), C17(H17), C216(H216),
 C18(H18), C303(H303), C2(H2), C217(H217), C205(H205), C321(H321), C204(H204),
 C323(H323), C322(H322), C315(H315), C324(H324), C118(H118), C312(H312),
 C304(H304), C202(H202), C102(H102), C112(H112), C208(H208), C317(H317),
 C107(H107), C316(H316), C308(H308), C103(H103), C212(H212), C203(H203),
 C108(H108), C117(H117), C306(H306), C305(H305), C309(H309), C209(H209),
 C210(H210), C113(H113), C311(H311), C310(H310), C211(H211)
2.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C22(H22A,H22B,H22C), C21(H21A,H21B,H21C), C128(H12A,H12B,
 H12C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C),
 C127(H12D,H12E,H12F), C124(H12G,H12H,H12I), C28(H28A,H28B,H28C), C123(H12J,
 H12K,H12L), C27(H27A,H27B,H27C), C122(H12M,H12N,H12O), C121(H12P,H12Q,H12R),
 C126(H12S,H12T,H12U), C125(H12V,H12W,H12X)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              40455
_shelx_hkl_checksum              43354
_shelx_fab_checksum              31100
_olex2_submission_special_instructions 'No special instructions were received'