Magnetic and thermodynamic control of coordination network crystallization using a hexaazaphenalene-based ligand.
Jiang, Qiao; Suzuki, Hiroaki; Wada, Yuki; Wang, Xiaohan; Murakami, Yoichi; Matsumoto, Takaya; Usov, Pavel M.; Kawano, Masaki; Chemical communications (Cambridge, England) 60 (2024) 8236–8239; doi:10.1039/d4cc01951b

data_7133308
_publ_section_title
;
 Magnetic and thermodynamic control of coordination network
 crystallization using a hexaazaphenalene-based ligand.
;
_journal_issue                   63
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              8236
_journal_page_last               8239
_journal_paper_doi               10.1039/d4cc01951b
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety
'C46.817 H34.451 Cd2 N18 O4, 2(Cl O4), 4.523(O), 4.857(C O), 2(C O0.333)'
_chemical_formula_sum            'C53.67 H34.45 Cd2 Cl2 N18 O22.05'
_chemical_formula_weight         1579.98
_chemical_name_common            Cd-4TPHAP-1
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-03-11
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-03-11 deposited with the CCDC.	2024-07-10 downloaded from the CCDC.
;
_cell_angle_alpha                80.3950(10)
_cell_angle_beta                 84.2250(10)
_cell_angle_gamma                78.4430(10)
_cell_formula_units_Z            1
_cell_length_a                   11.81030(10)
_cell_length_b                   12.5965(2)
_cell_length_c                   13.3862(2)
_cell_measurement_reflns_used    22935
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      75.2640
_cell_measurement_theta_min      3.3440
_cell_volume                     1919.06(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      123.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_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  26.00   0.50    0.05    --  -48.44  19.00-120.00   56
  2  \w    -27.00  24.00   0.50    0.05    --  -48.44  37.00 -30.00  102
  3  \w     -6.00  19.00   0.50    0.05    --  -48.44  19.00 -30.00   50
  4  \w     -6.00  24.00   0.50    0.05    --  -48.44  19.00   0.00   60
  5  \w     -6.00  20.00   0.50    0.05    --  -48.44  19.00 120.00   52
  6  \w     -6.00  24.00   0.50    0.05    --  -48.44  19.00 -90.00   60
  7  \w     32.00  79.00   0.50    0.10    --  102.75 -61.00 -60.00   94
  8  \w     33.00  64.00   0.50    0.10    --  102.75 -61.00 150.00   62
  9  \w     87.00 113.00   0.50    0.10    --  102.75 -77.00 -90.00   52
 10  \w     32.00  70.00   0.50    0.10    --  102.75 -77.00 -90.00   76
 11  \w     35.00  60.00   0.50    0.10    --  102.75 -61.00-180.00   50
 12  \w     58.00  84.00   0.50    0.10    --  102.75 -83.00-119.00   52
 13  \w     76.00 102.00   0.50    0.10    --  102.75-125.00-120.00   52
 14  \w     36.00  69.00   0.50    0.10    --  102.75-125.00-120.00   66
 15  \w     39.00  91.00   0.50    0.10    --  102.75-125.00-150.00  104
 16  \w     34.00 110.00   0.50    0.10    --  102.75-125.00  60.00  152
 17  \w     72.00  97.00   0.50    0.10    --  102.75-125.00  90.00   50
 18  \w     47.00  73.00   0.50    0.10    --  102.75-125.00 150.00   52
 19  \w     34.00 103.00   0.50    0.10    --  102.75-125.00 120.00  138
 20  \w     40.00 106.00   0.50    0.10    --  102.75 -98.00  99.88  132
 21  \w     31.00 103.00   0.50    0.10    --  102.75 -94.00 120.00  144
 22  \w     58.00 103.00   0.50    0.10    --  102.75 -94.00  60.00   90
 23  \w     61.00  96.00   0.50    0.10    --  102.75 -94.00 150.00   70
 24  \w     37.00  67.00   0.50    0.10    --  102.75 -94.00 -90.00   60
 25  \w     31.00  57.00   0.50    0.10    --  102.75 -94.00-150.00   52
 26  \w     61.00  88.00   0.50    0.10    --  102.75 -94.00-150.00   54
 27  \w    -23.00  58.00   0.50    0.05    --   48.44 -83.00-119.00  162
 28  \w     33.00 106.00   0.50    0.10    --  102.75 -94.00 -60.00  146
 29  \w     60.00  89.00   0.50    0.10    --  102.75 -94.00   0.00   58
 30  \w     98.00 173.00   0.50    0.10    --  102.75  30.00 -60.00  150
 31  \w     92.00 171.00   0.50    0.10    --  102.75  45.00 -30.00  158
 32  \w     94.00 159.00   0.50    0.10    --  102.75  45.00  60.00  130
 33  \w    144.00 169.00   0.50    0.10    --  102.75  30.00  30.00   50
 34  \w    136.00 165.00   0.50    0.10    --  102.75  77.00 120.00   58
 35  \w     92.00 174.00   0.50    0.10    --  102.75  45.00 150.00  164
 36  \w     86.00 111.00   0.50    0.10    --  102.75  77.00 120.00   50
 37  \w     40.00 116.00   0.50    0.05    --   48.44  37.00  30.00  152
 38  \w     94.00 119.00   0.50    0.10    --  102.75  30.00  30.00   50
 39  \w     85.00 174.00   0.50    0.10    --  102.75  83.00   2.00  178
 40  \w    -25.00   0.00   0.50    0.05    --   48.44 -19.00 -90.00   50
 41  \w    -25.00   0.00   0.50    0.05    --   48.44 -19.00 120.00   50
 42  \w   -125.00 -99.00   0.50    0.10    -- -102.00 143.00 126.98   52
 43  \w   -125.00 -94.00   0.50    0.10    -- -102.00 143.00 168.35   62
 44  \w    -60.00 -33.00   0.50    0.10    -- -102.00 143.00 168.35   54
 45  \w   -121.00 -89.00   0.50    0.10    -- -102.00 139.00 -13.12   64
 46  \w   -106.00 -80.00   0.50    0.10    -- -102.00 103.00  14.21   52
 47  \w    -59.00 -33.00   0.50    0.10    -- -102.00 103.00  14.21   52
 48  \w    -76.00 -44.00   0.50    0.10    -- -102.00  83.00   2.00   64
 49  \w    -62.00 -36.00   0.50    0.10    -- -102.00 107.00-110.68   52
 50  \w   -122.00 -83.00   0.50    0.10    -- -102.00 140.00-116.19   78
 51  \w   -107.00 -80.00   0.50    0.10    -- -102.00 107.00-110.68   54
 52  \w    -60.00 -31.00   0.50    0.10    -- -102.00  61.00-180.00   58
 53  \w    -73.00 -30.00   0.50    0.10    -- -102.00  61.00-150.00   86
 54  \w   -175.00-125.00   0.50    0.10    -- -102.00 -30.00 -60.00  100
 55  \w   -142.00 -80.00   0.50    0.10    -- -102.00 -83.00-119.00  124
 56  \w   -175.00 -92.00   0.50    0.10    -- -102.00 -30.00  90.00  166
 57  \w    -72.00  24.00   0.50    0.05    --  -48.44  83.00   2.00  192
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0034332000
_diffrn_orient_matrix_UB_12      -0.0999279000
_diffrn_orient_matrix_UB_13      -0.0534926000
_diffrn_orient_matrix_UB_21      0.0657298000
_diffrn_orient_matrix_UB_22      -0.0750005000
_diffrn_orient_matrix_UB_23      0.0870332000
_diffrn_orient_matrix_UB_31      -0.1161059000
_diffrn_orient_matrix_UB_32      -0.0182563000
_diffrn_orient_matrix_UB_33      0.0570447000
_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  0.0534
_diffrn_reflns_av_unetI/netI     0.0438
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            35291
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.121
_diffrn_reflns_theta_min         4.555
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.740
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70139
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'yellowish colourless'
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             789
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.075
_refine_diff_density_max         1.622
_refine_diff_density_min         -1.210
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     565
_refine_ls_number_reflns         7898
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0522
_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^)+(0.1062P)^2^+1.5846P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1464
_refine_ls_wR_factor_ref         0.1500
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7231
_reflns_number_total             7898
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01951b2.cif
_cod_data_source_block           Cd-4TPHAP-1
_cod_depositor_comments
'Adding full bibliography for 7133308--7133309.cif.'
_cod_database_code               7133308
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CdCHNO
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O6S-C5S \\sim O4S-C3S
 with sigma of 0.02
 Cl38-O42 \\sim Cl38-O43
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C9S \\sim O10S: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
Uanis(O35) = Uanis(O33)
4. Others
 1*[Sof(O4W)]+1*[Sof(O6W)]+1*[Sof(O7W)]+1*[Sof(O5W)]=1 with esd of 0.01
 Sof(O1W)=1-FVAR(1)
 Sof(O2S)=Sof(C1S)=FVAR(1)
 Sof(O3W)=1-FVAR(2)
 Sof(O12S)=Sof(C11S)=FVAR(2)
 Sof(O4S)=Sof(C3S)=1-FVAR(3)
 Sof(O6S)=Sof(C5S)=FVAR(3)
 Sof(O33)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=1-FVAR(8)
 Sof(O35)=FVAR(8)
 Fixed Sof: O42(0.5) O8S(0.333333) C7S(0.333333) O2W(0.333333) O10S(0.333333)
 O43(0.5)
5.a Me refined with riding coordinates:
 C34(H34A,H34B,H34C)
5.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C28(H28), C18(H18), C7(H7), C17(H17), C14(H14), C24(H24), C4(H4),
 C27(H27), C3(H3), C15(H15), C25(H25)
5.c Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C)
;
_shelx_res_checksum              95483
_shelx_hkl_checksum              22920
_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 1.497
_oxdiff_exptl_absorpt_empirical_full_min 0.739