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_7133309
_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
'C45.495 H31.486 Cd N18 O3, 10.17(O), 3.726(C O)'
_chemical_formula_sum            'C49.22 H31.49 Cd N18 O16.9'
_chemical_formula_weight         1257.77
_chemical_name_common            Cd-4TPHAP
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.3621(3)
_cell_length_b                   7.96360(10)
_cell_length_c                   28.1930(2)
_cell_measurement_reflns_used    17164
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      75.9210
_cell_measurement_theta_min      2.8360
_cell_volume                     6816.83(12)
_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 0.998
_diffrn_measured_fraction_theta_max 0.981
_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     34.00 106.00   0.50    0.48    --  102.75-125.00-180.00  144
  2  \w     40.00 106.00   0.50    0.48    --  102.75 -94.00  90.00  132
  3  \w     -6.00  26.00   0.50    0.48    --  -48.44  19.00  60.00   64
  4  \w     -4.00  26.00   0.50    0.48    --  -48.44  19.00  30.00   60
  5  \w    -60.00  24.00   0.50    0.48    --  -48.44  68.00 -81.00  168
  6  \w    -68.00 -43.00   0.50    0.48    -- -102.00  61.00-120.00   50
  7  \w    -74.00 -49.00   0.50    0.48    -- -102.00  61.00 -90.00   50
  8  \w    -74.00 -49.00   0.50    0.48    -- -102.00  61.00  30.00   50
  9  \w    -60.00 -31.00   0.50    0.48    -- -102.00  61.00 120.00   58
 10  \w   -174.00 -95.00   0.50    0.48    -- -102.00 -73.00 -87.00  158
 11  \w     31.00  67.00   0.50    0.48    --  102.75 -61.00-150.00   72
 12  \w     44.00 102.00   0.50    0.48    --  102.75 -80.00  30.00  116
 13  \w    -22.00   6.00   0.50    0.48    --   48.44 -19.00 150.00   56
 14  \w     34.00  78.00   0.50    0.48    --  102.75 -61.00  60.00   88
 15  \w     46.00  71.00   0.50    0.48    --  102.75 -68.00 145.00   50
 16  \w    117.00 167.00   0.50    0.48    --  102.75  45.00  90.00  100
 17  \w    138.00 172.00   0.50    0.48    --  102.75  61.00  60.00   68
;
_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      0.0019320000
_diffrn_orient_matrix_UB_12      0.1450737000
_diffrn_orient_matrix_UB_13      0.0360782000
_diffrn_orient_matrix_UB_21      -0.0435370000
_diffrn_orient_matrix_UB_22      -0.0608014000
_diffrn_orient_matrix_UB_23      0.0222071000
_diffrn_orient_matrix_UB_31      0.0260274000
_diffrn_orient_matrix_UB_32      -0.1124712000
_diffrn_orient_matrix_UB_33      0.0345215000
_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  0.0388
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            36119
_diffrn_reflns_point_group_measured_fraction_full 0.800
_diffrn_reflns_point_group_measured_fraction_max 0.764
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.102
_diffrn_reflns_theta_min         5.536
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.180
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86824
_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    1.226
_exptl_crystal_description       prism
_exptl_crystal_F_000             2544
_exptl_crystal_size_max          0.205
_exptl_crystal_size_mid          0.175
_exptl_crystal_size_min          0.095
_refine_diff_density_max         0.631
_refine_diff_density_min         -0.789
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
;
 Flack x determined using 2844 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.014(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     980
_refine_ls_number_reflns         10872
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0539
_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^)+(0.1209P)^2^+1.1780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1509
_refine_ls_wR_factor_ref         0.1593
_reflns_Friedel_coverage         0.525
_reflns_Friedel_fraction_full    0.593
_reflns_Friedel_fraction_max     0.538
_reflns_number_gt                9490
_reflns_number_total             10872
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01951b2.cif
_cod_data_source_block           Cd-4TPHAP-2
_cod_depositor_comments
'Adding full bibliography for 7133308--7133309.cif.'
_cod_original_formula_sum        'C49.22 H31.49 Cd N18 O16.90'
_cod_database_code               7133309
_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, All O(H,H) groups
2. Restrained distances
 O1L-H1L
 0.87 with sigma of 0.01
 C2L-H1L
 1.874078 with sigma of 0.02
 Cd1-H1L
 2.873715 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O8W) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O16W) \\sim Ueq, Uanis(O12W) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
4. Others
 Sof(C2C)=Sof(H2C)=Sof(C3C)=Sof(H3C)=Sof(C5C)=Sof(H5C)=Sof(C6C)=Sof(H6C)=
 Sof(O3W)=Sof(O6W)=Sof(O12W)=1-FVAR(1)
 Sof(C2B)=Sof(H2B)=Sof(C3B)=Sof(H3B)=Sof(C5B)=Sof(H5B)=Sof(C6B)=Sof(H6B)=
 Sof(O2W)=Sof(O7W)=Sof(O9W)=FVAR(1)
 Sof(O11W)=1-FVAR(2)
 Sof(C5S)=Sof(O6S)=FVAR(2)
 Sof(O20W)=1-FVAR(3)
 Sof(C1S)=Sof(O2S)=FVAR(3)
 Sof(C5L)=Sof(H5LA)=Sof(H5LB)=Sof(H5LC)=Sof(O21W)=Sof(O18W)=1-FVAR(4)
 Sof(O1W)=Sof(O19W)=FVAR(4)
 Sof(C3S)=Sof(O4S)=FVAR(5)
 Sof(C7S)=Sof(O8S)=FVAR(6)
 Sof(C1)=Sof(H1)=Sof(C2)=Sof(H2)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=1-FVAR(7)
 Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=Sof(C26A)=Sof(H26A)=Sof(C27A)=
 Sof(H27A)=FVAR(7)
 Fixed Sof: O10W(0.25) O16W(0.25) O17W(0.25)
5.a Rotating group:
 O3L(H3LA,H3LB)
5.b Me refined with riding coordinates:
 C2L(H2LA,H2LB,H2LC)
5.c Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C3A(H3A), C5A(H5A), C6A(H6A), C13A(H13A), C14A(H14A), C16A(H16A),
 C17A(H17A), C23A(H23A), C24A(H24A), C26A(H26A), C27A(H27A), C2B(H2B), C3B(H3B),
  C5B(H5B), C6B(H6B), C13B(H13B), C14B(H14B), C16B(H16B), C17B(H17B),
 C23B(H23B), C24B(H24B), C26B(H26B), C27B(H27B), C2C(H2C), C3C(H3C), C5C(H5C),
 C6C(H6C), C1(H1), C2(H2), C3(H3), C4(H4)
5.d Idealised Me refined as rotating group:
 C5L(H5LA,H5LB,H5LC)
;
_shelx_res_checksum              87578
_shelx_hkl_checksum              26732
_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 1.211
_oxdiff_exptl_absorpt_empirical_full_min 0.823