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_7720865
_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_formula_moiety         'C52 H46 Ga4 N4 O8, 5(C H2 Cl2)'
_chemical_formula_sum            'C57 H56 Cl10 Ga4 N4 O8'
_chemical_formula_weight         1558.43
_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
_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                102.112(19)
_cell_angle_beta                 107.393(18)
_cell_angle_gamma                101.202(17)
_cell_formula_units_Z            1
_cell_length_a                   10.2423(18)
_cell_length_b                   12.817(3)
_cell_length_c                   15.306(3)
_cell_measurement_reflns_used    1484
_cell_measurement_temperature    100.01(11)
_cell_measurement_theta_max      59.6520
_cell_measurement_theta_min      4.7100
_cell_volume                     1802.2(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 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_environment      N~2~
_diffrn_ambient_temperature      100.01(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2974
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.947
_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      2.00  98.00   1.00    7.50    --   31.92  77.00-180.00   96
  2  \w      1.00  70.00   1.00    7.50    --   31.92 -99.00-120.00   69
  3  \w     37.00 100.00   1.00    7.50    --   31.92  57.00 -60.00   63
  4  \w    -23.00   5.00   1.00    7.50    --   31.92 -57.00 -60.00   28
  5  \w    -35.00  56.00   1.00    7.50    --   31.92 -77.00  60.00   91
  6  \w      9.00  52.00   1.00    7.50    --   31.92 -57.00 -60.00   43
  7  \w     59.00  87.00   1.00    7.50    --   31.92  57.00  30.00   28
  8  \w     26.00 111.00   1.00   32.00    --   89.35 -61.00  60.00   85
  9  \w    108.00 145.00   1.00   32.00    --   89.35 111.00-180.00   37
 10  \w     44.00 102.00   1.00   32.00    --   89.35 -94.00  30.00   58
 11  \w     65.00 109.00   1.00   32.00    --   89.35-111.00 -30.00   44
 12  \w    111.00 150.00   1.00   32.00    --   89.35 178.00 -90.00   39
 13  \w    106.00 162.00   1.00   32.00    --   89.35 111.00 120.00   56
 14  \w    104.00 159.00   1.00   32.00    --   89.35 111.00  90.00   55
 15  \w     18.00 117.00   1.00   32.00    --   89.35 -30.00 150.00   99
 16  \w     64.00 131.00   1.00   32.00    --   89.35  30.00-180.00   67
 17  \w     78.00 138.00   1.00   32.00    --   89.35  45.00  30.00   60
 18  \w     20.00 117.00   1.00   32.00    --   89.35 -77.00-180.00   97
 19  \w     66.00 105.00   1.00   32.00    --   89.35 178.00  30.00   39
 20  \w    119.00 144.00   1.00   32.00    --   89.35 178.00  30.00   25
 21  \w     36.00 128.00   1.00   32.00    --   89.35  15.00 150.00   92
;
_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      -0.0935999000
_diffrn_orient_matrix_UB_12      -0.0961980000
_diffrn_orient_matrix_UB_13      -0.0899157000
_diffrn_orient_matrix_UB_21      -0.0579899000
_diffrn_orient_matrix_UB_22      -0.0625529000
_diffrn_orient_matrix_UB_23      0.0621496000
_diffrn_orient_matrix_UB_31      -0.1214861000
_diffrn_orient_matrix_UB_32      0.0564412000
_diffrn_orient_matrix_UB_33      -0.0130030000
_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  0.1362
_diffrn_reflns_av_unetI/netI     0.1632
_diffrn_reflns_Laue_measured_fraction_full 0.947
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8871
_diffrn_reflns_point_group_measured_fraction_full 0.947
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        61.482
_diffrn_reflns_theta_max         61.482
_diffrn_reflns_theta_min         3.669
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.518
_exptl_absorpt_correction_T_max  0.896
_exptl_absorpt_correction_T_min  0.706
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_description       plate
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.756
_refine_diff_density_min         -1.664
_refine_diff_density_rms         0.263
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.491
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         5301
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.497
_refine_ls_R_factor_all          0.2320
_refine_ls_R_factor_gt           0.1792
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_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          0.4417
_refine_ls_wR_factor_ref         0.4768
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3114
_reflns_number_total             5301
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00374e2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7720862--7720867.cif.'
_cod_original_cell_volume        1802.3(7)
_cod_database_code               7720865
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C40 H30 O4 Al2 N2'
_reflns_odcompleteness_completeness 98.32
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     58.86
_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. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C18)
\\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C25) \\sim Ueq,
Uanis(C27) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O4)
\\sim Ueq, Uanis(N2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.01
3. Others
 Fixed Sof: Cl5(0.5) Cl6(0.5) C29(0.5) H29A(0.5) H29B(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C27(H27A,H27B), C29(H29A,H29B)
4.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C10(H10), C11(H11), C12(H12), C14(H14), C17(H17), C21(H21),
 C26(H26), C22(H22), C23(H23)
4.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C)
;
_shelx_res_checksum              504
_shelx_hkl_checksum              20583
_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 5.299
_oxdiff_exptl_absorpt_empirical_full_min 0.218