Structural diversity of dimethylgallium naphthalene-2,3-dicarboxylate/pyridine systems
Solka, Maksymilian; Terlecki, Michał; Justyniak, Iwona; Ziemkowska, Wanda; Prochowicz, Daniel; Lewinski, Janusz; Dalton Transactions  (2026) –; doi:10.1039/D6DT00374E

data_7720867
_publ_section_title
;
 Structural diversity of dimethylgallium
 naphthalene-2,3-dicarboxylate/pyridine systems.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7709
_journal_page_last               7717
_journal_paper_doi               10.1039/d6dt00374e
_journal_volume                  55
_journal_year                    2026
_chemical_absolute_configuration rm
_chemical_formula_moiety
'3(C58 H72 Al2 Ga2 N4 O6), C58 H70 Al2 Ga2 N4 O6, 6(C7 H8)'
_chemical_formula_sum            'C274 H334 Al8 Ga8 N16 O24'
_chemical_formula_weight         5009.15
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2026-02-07
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2026-02-11 deposited with the CCDC.	2026-04-10 downloaded from the CCDC.
;
_cell_angle_alpha                83.921(3)
_cell_angle_beta                 75.537(3)
_cell_angle_gamma                71.123(3)
_cell_formula_units_Z            1
_cell_length_a                   14.0030(4)
_cell_length_b                   20.4774(7)
_cell_length_c                   26.4863(10)
_cell_measurement_reflns_used    17829
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      69.7880
_cell_measurement_theta_min      3.4260
_cell_volume                     6956.0(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2974
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     46.00  73.20   0.85    7.00    --    0.00  19.00  30.00   32
  2  \w    -21.00  19.80   0.85    7.00    --    0.00 -77.00-150.00   48
  3  \w    -35.00  33.00   0.85    7.00    --    0.00  19.00  30.00   80
  4  \w      0.00  27.20   0.85    7.00    --    0.00 -77.00   0.00   32
  5  \w     -2.00  33.70   0.85    7.00    --    0.00  77.00 120.00   42
  6  \w     39.00 122.30   0.85   22.50    --   54.00  57.00 -30.00   98
  7  \w     36.00 102.30   0.85   22.50    --   54.00  57.00 120.00   78
  8  \w      8.00  95.55   0.85   22.50    --   54.00 -99.00 -90.00  103
  9  \w     73.00 115.50   0.85   22.50    --   54.00  37.00 -90.00   50
 10  \w     50.00  90.80   0.85   22.50    --   54.00-125.00 150.00   48
 11  \w     72.00 114.50   0.85   22.50    --   54.00  57.00-150.00   50
 12  \w     -5.00  57.90   0.85   22.50    --   54.00 -57.00 150.00   74
 13  \w     -7.00  64.40   0.85   22.50    --   54.00 -57.00   0.00   84
 14  \w     77.00 104.20   0.85   52.50    --  108.00-111.00  30.00   32
 15  \w     36.00  63.20   0.85   52.50    --  108.00-111.00-120.00   32
 16  \w    125.00 177.70   0.85   52.50    --  108.00  25.00 -90.00   62
 17  \w     83.00 122.10   0.85   52.50    --  108.00  25.00 -90.00   46
 18  \w    124.00 166.50   0.85   52.50    --  108.00  77.00 -90.00   50
 19  \w     38.00  77.10   0.85   52.50    --  108.00 -91.00  90.00   46
 20  \w     81.00 106.50   0.85   52.50    --  108.00-111.00-150.00   30
 21  \w     41.00  68.20   0.85   52.50    --  108.00-111.00-150.00   32
 22  \w     43.00 128.85   0.85   52.50    --  108.00 -63.00 120.00  101
 23  \w     80.00 107.20   0.85   52.50    --  108.00-111.00 -60.00   32
 24  \w     42.00 130.40   0.85   52.50    --  108.00 -37.00 -30.00  104
 25  \w     83.00 133.15   0.85   52.50    --  108.00  37.00  30.00   59
 26  \w     36.00 132.90   0.85   52.50    --  108.00 -37.00-150.00  114
 27  \w     38.00 108.55   0.85   52.50    --  108.00-111.00 150.00   83
 28  \w     48.00 108.35   0.85   52.50    --  108.00-111.00  60.00   71
 29  \w     81.00 106.50   0.85   52.50    --  108.00-111.00-120.00   30
 30  \w     45.00 137.65   0.85   52.50    --  108.00 -77.00-120.00  109
 31  \w     36.00 168.60   0.85   52.50    --  108.00  12.00-120.00  156
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0118990000
_diffrn_orient_matrix_UB_12      -0.0384202000
_diffrn_orient_matrix_UB_13      -0.0492593000
_diffrn_orient_matrix_UB_21      0.1151865000
_diffrn_orient_matrix_UB_22      -0.0365583000
_diffrn_orient_matrix_UB_23      -0.0004364000
_diffrn_orient_matrix_UB_31      -0.0292960000
_diffrn_orient_matrix_UB_32      -0.0592742000
_diffrn_orient_matrix_UB_33      0.0344167000
_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  0.0565
_diffrn_reflns_av_unetI/netI     0.0713
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            50543
_diffrn_reflns_point_group_measured_fraction_full 0.625
_diffrn_reflns_point_group_measured_fraction_max 0.610
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.153
_diffrn_reflns_theta_min         2.821
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.584
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_T_min  0.927
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_description       plate
_exptl_crystal_F_000             2634
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.790
_refine_diff_density_min         -1.368
_refine_diff_density_rms         0.117
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.06(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3009
_refine_ls_number_reflns         32270
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.1173
_refine_ls_R_factor_gt           0.0961
_refine_ls_shift/su_max          0.081
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2596
_refine_ls_wR_factor_ref         0.2798
_reflns_Friedel_coverage         0.250
_reflns_Friedel_fraction_full    0.256
_reflns_Friedel_fraction_max     0.244
_reflns_number_gt                25099
_reflns_number_total             32270
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00374e2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7720862--7720867.cif.'
_cod_database_code               7720867
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C40 H40 O4 N4 Al2 Ga2'
_reflns_odcompleteness_completeness 99.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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:
 C02O(H02O), C9(H9), C19(H19), C020(H020), C21(H21), C25(H25), C28(H28),
 C40(H40), C42(H42), C44(H44), C77(H77), C79(H79), C83(H83), C86(H86), C99(H99),
  C101(H101), C126(H126), C138(H138), C140(H140), C142(H142), C184(H184),
 C194(H194), C196(H196), C200(H200), C203(H203), C213(H213), C215(H215),
 C219(H219), C311(H311), C319(H319)
2.b Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C38(H38A,
 H38B), C39(H39A,H39B), C41(H41A,H41B), C43(H43A,H43B), C064(H06A,H06B),
 C78(H78A,H78B), C80(H80A,H80B), C81(H81A,H81B), C82(H82A,H82B), C97(H97A,H97B),
  C98(H98A,H98B), C100(H10A,H10B), C102(H10C,H10D), C136(H13A,H13B), C137(H13C,
 H13D), C139(H13E,H13F), C141(H14A,H14B), C195(H19A,H19B), C197(H19C,H19D),
 C198(H19E,H19F), C199(H19G,H19H), C214(H21A,H21B), C216(H21C,H21D), C217(H21E,
 H21F), C218(H21G,H21H), C313(H31A,H31B), C315(H31C,H31D), C318(H31E,H31F)
2.c Aromatic/amide H refined with riding coordinates:
 C02N(H02N), C11(H11), C12(H12), C14(H14), C15(H15), C16(H16), C17(H17),
 C023(H023), C26(H26), C30(H30), C31(H31), C33(H33), C34(H34), C35(H35),
 C36(H36), C45(H45), C49(H49), C050(H050), C51(H51), C53(H53), C54(H54),
 C055(H055), C56(H56), C69(H69), C70(H70), C72(H72), C73(H73), C74(H74),
 C75(H75), C84(H84), C086(H086), C88(H88), C89(H89), C92(H92), C93(H93),
 C94(H94), C95(H95), C104(H104), C108(H108), C110(H110), C111(H111), C112(H112),
  C113(H113), C115(H115), C128(H128), C129(H129), C131(H131), C132(H132),
 C133(H133), C134(H134), C143(H143), C186(H186), C187(H187), C189(H189),
 C190(H190), C191(H191), C192(H192), C201(H201), C205(H205), C206(H206),
 C208(H208), C209(H209), C210(H210), C211(H211), C220(H220), C224(H224),
 C226(H226), C227(H227), C228(H228), C229(H229), C231(H231), C236(H236),
 C237(H237), C238(H238), C239(H239), C240(H240), C243(H243), C244(H244),
 C245(H245), C246(H246), C247(H247), C257(H257), C258(H258), C259(H259),
 C260(H260), C261(H261), C264(H264), C265(H265), C266(H266), C268(H268),
 C270(H270), C271(H271), C273(H273), C274(H274), C278(H278), C279(H279),
 C280(H280), C281(H281), C282(H282), C309(H309), C310(H310), C312(H312),
 C316(H316), C317(H317), C323(H323), C324(H324), C325(H325), C553(H553),
 C267(H267), C272(H272)
2.d X=CH2 refined with riding coordinates:
 C27(H27A,H27B), C46(H46A,H46B), C070(H07A,H07B), C85(H85A,H85B), C105(H10E,
 H10F), C144(H14C,H14D), C202(H20C,H20D), C221(H22C,H22D)
2.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,
 H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C59(H59A,H59B,
 H59C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C), C63(H63A,
 H63B,H63C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C),
 C118(H11A,H11B,H11C), C119(H11D,H11E,H11F), C120(H12A,H12B,H12C), C121(H12D,
 H12E,H12F), C122(H12G,H12H,H12I), C123(H12J,H12K,H12L), C124(H12M,H12N,H12O),
 C125(H12P,H12Q,H12R), C176(H17A,H17B,H17C), C177(H17D,H17E,H17F), C178(H17G,
 H17H,H17I), C179(H17J,H17K,H17L), C180(H18A,H18B,H18C), C181(H18D,H18E,H18F),
 C182(H18G,H18H,H18I), C183(H18J,H18K,H18L), C234(H23C,H23D,H23E), C241(H24C,
 H24D,H24E), C255(H25A,H25B,H25C), C262(H26A,H26B,H26C), C276(H27C,H27D,H27E),
 C288(H28A,H28B,H28C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              42952
_shelx_hkl_checksum              48415
_shelx_fab_checksum              82194
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.773
_oxdiff_exptl_absorpt_empirical_full_min 0.420