Synthesis, structure, and properties of helical bis-Zn(ii) complexes of hexapyrrolic ligands
Chauhan, Pinky; Pushpanandan, Poornenth; Ravikanth, Mangalampalli; CrystEngComm 26 (2024) 2259–2268; doi:10.1039/D4CE00019F

data_7248334
_publ_section_title
;
 Synthesis, structure, and properties of helical bis-Zn(ii) complexes of
 hexapyrrolic ligands
;
_journal_issue                   17
_journal_name_full               CrystEngComm
_journal_page_first              2259
_journal_page_last               2268
_journal_paper_doi               10.1039/D4CE00019F
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C86 H72 N12 Zn2'
_chemical_formula_sum            'C86 H72 N12 Zn2'
_chemical_formula_weight         1404.29
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-06-12
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2023-10-09 deposited with the CCDC.	2024-03-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3533(4)
_cell_length_b                   27.6883(8)
_cell_length_c                   21.4440(7)
_cell_measurement_reflns_used    4385
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      23.6990
_cell_measurement_theta_min      1.7980
_cell_volume                     7334.7(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f     36.25 184.00   0.75   10.00  31.10 -18.16 -31.50    --   197
  2  \w   -122.88  22.62   0.75   10.00    --  -18.16 -59.25  20.08  194
  3  \w    -76.15   6.35   0.75   10.00    --  -18.16  89.85 -32.67  110
  4  \f   -120.30  10.95   0.75   10.00  72.70 -18.16  31.50    --   175
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0036057000
_diffrn_orient_matrix_UB_12      -0.0096776000
_diffrn_orient_matrix_UB_13      0.0305488000
_diffrn_orient_matrix_UB_21      -0.0317910000
_diffrn_orient_matrix_UB_22      -0.0193635000
_diffrn_orient_matrix_UB_23      -0.0115206000
_diffrn_orient_matrix_UB_31      0.0477043000
_diffrn_orient_matrix_UB_32      -0.0136665000
_diffrn_orient_matrix_UB_33      -0.0053590000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1461
_diffrn_reflns_av_unetI/netI     0.0720
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            64504
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.805
_diffrn_source                   'sealed tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.708
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47655
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_description       needle
_exptl_crystal_F_000             2928
_exptl_crystal_size_max          0.189
_exptl_crystal_size_mid          0.156
_exptl_crystal_size_min          0.086
_refine_diff_density_max         0.404
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         6457
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0541
_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^)+(0.0583P)^2^+6.5641P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1256
_refine_ls_wR_factor_ref         0.1481
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4374
_reflns_number_total             6457
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00019f2.cif
_cod_data_source_block           mr_pc_zn3_autored_sq
_cod_depositor_comments          'Adding full bibliography for 7248334.cif.'
_cod_database_code               7248334
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.942
_shelx_estimated_absorpt_t_min   0.878
_reflns_odcompleteness_completeness 91.01
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.12
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N004(H004), N008(H008), C00J(H00J), C00M(H00M), C00N(H00N), C00Q(H00Q),
 C00R(H00R), C00U(H00U), C00V(H00V), C00W(H00W), C00Y(H00Y), C00Z(H00Z),
 C010(H010), C011(H011), C012(H012), C014(H014), C015(H015), C016(H016),
 C017(H017), C019(H019), C01A(H01D), C01B(H01E), C01C(H01F), C01E(H01J)
2.b Idealised Me refined as rotating group:
 C013(H01A,H01B,H01C), C01D(H01G,H01H,H01I), C01F(H01K,H01L,H01M), C01G(H01N,
 H01O,H01P)
;
_shelx_res_checksum              22585
_shelx_fab_checksum              79511
_platon_squeeze_void_probe_radius 1.20
_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 1.827
_oxdiff_exptl_absorpt_empirical_full_min 0.551