Steric control of mesocate and helicate formation: Bulky pyrrol-2-yl Schiff base complexes of Zn2+
Niklas, J.E.; Hiti, E.A.; Wilkinson, G.R.; Mayhugh, J.T.; Gorden, J.D.; Gorden, A.E.V.; Inorganica Chimica Acta 529 (2022) 120653–; doi:10.1016/j.ica.2021.120653

data_1566015
_publ_section_title
;
 Steric control of mesocate and helicate formation: Bulky pyrrol-2-yl
 Schiff base complexes of Zn2+
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              120653
_journal_paper_doi               10.1016/j.ica.2021.120653
_journal_volume                  529
_journal_year                    2022
_chemical_formula_moiety         'C152 H136 N16 O16 Zn4'
_chemical_formula_sum            'C152 H136 N16 O16 Zn4'
_chemical_formula_weight         2704.33
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_symmetry_Int_Tables_number      88
_atom_sites_solution_primary     iterative
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.2528(2)
_cell_length_b                   24.2528(2)
_cell_length_c                   27.6148(7)
_cell_measurement_reflns_used    14561
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.4490
_cell_measurement_theta_min      2.4070
_cell_volume                     16243.0(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XH (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9962
_diffrn_measured_fraction_theta_max 0.9962
_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     -4.00  52.00   0.50    8.61    --   18.43 -99.00  30.00  112
  2  \w     65.00 102.00   0.50   25.00    --  110.00-111.00-132.00   74
  3  \w     73.00 101.00   0.50   25.00    --  110.00 -95.00 -90.00   56
  4  \w     45.00 133.00   0.50   25.00    --  110.00 -77.00 -30.00  176
  5  \w     91.00 117.00   0.50   25.00    --  110.00  15.00  30.00   52
  6  \w    134.00 159.00   0.50   25.00    --  110.00  15.00  30.00   50
  7  \w     84.00 176.00   0.50   25.00    --  110.00  79.00  74.00  184
  8  \w    123.00 176.00   0.50   25.00    --  110.00 125.00  30.00  106
  9  \w    111.00 139.00   0.50   25.00    --  110.00  46.00-117.00   56
 10  \w     49.00  90.00   0.50    8.61    --   18.43  57.00 -90.00   82
 11  \w     -3.00  83.00   0.50    8.61    --   18.43  79.00  74.00  172
 12  \w     38.00 102.00   0.50   25.00    --  110.00 -95.00  90.00  128
 13  \w     34.00 128.00   0.50   25.00    --  110.00 -30.00 120.00  188
 14  \w     35.00  47.50   0.50   25.00    --  110.00 -30.00 -30.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0525321000
_diffrn_orient_matrix_UB_12      -0.0351950000
_diffrn_orient_matrix_UB_13      0.0052169000
_diffrn_orient_matrix_UB_21      -0.0119740000
_diffrn_orient_matrix_UB_22      0.0074623000
_diffrn_orient_matrix_UB_23      -0.0544288000
_diffrn_orient_matrix_UB_31      0.0335188000
_diffrn_orient_matrix_UB_32      -0.0523692000
_diffrn_orient_matrix_UB_33      -0.0112766000
_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  0.0329
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            34577
_diffrn_reflns_theta_full        70.0556
_diffrn_reflns_theta_max         70.06
_diffrn_reflns_theta_min         2.42
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.147
_exptl_absorpt_correction_T_max  0.776
_exptl_absorpt_correction_T_min  0.672
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.20a (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.1058
_exptl_crystal_description       block
_exptl_crystal_F_000             5623.1202
_exptl_crystal_size_max          0.497
_exptl_crystal_size_mid          0.324
_exptl_crystal_size_min          0.221
_refine_diff_density_max         2.4510
_refine_diff_density_min         -0.4287
_refine_diff_density_rms         0.1266
_refine_ls_d_res_high            0.8201
_refine_ls_d_res_low             18.2227
_refine_ls_goodness_of_fit_ref   1.4752
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    70
_refine_ls_number_parameters     446
_refine_ls_number_reflns         7681
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.4607
_refine_ls_R_factor_all          0.1071
_refine_ls_R_factor_gt           0.0939
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2964
_refine_ls_wR_factor_ref         0.3395
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              29
_reflns_limit_h_min              0
_reflns_limit_k_max              29
_reflns_limit_k_min              0
_reflns_limit_l_max              33
_reflns_limit_l_min              0
_reflns_number_gt                5855
_reflns_number_total             7681
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ICA-2022-529-120653.cif
_cod_data_source_block           Zn4X4
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               1566015
_chemical_oxdiff_formula         C71N12O14Zn2
_reflns_odcompleteness_completeness 99.46
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_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. Rigid bond restraints
 C1, C10, C8, C1aa, C5aa, C3, C2aa, C2, C5, C4, C0aa, C6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C17, C3aa, C4aa, C31, C46, C33
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C6 \\sim C0aa \\sim C4 \\sim C5aa \\sim C1aa \\sim C8 \\sim C5 \\sim C3 \\sim
C2aa \\sim C2 \\sim C1 \\sim C10: within 1.7A with sigma of 0.02 and sigma for
terminal atoms of 0.04
C17 \\sim C3aa \\sim C4aa \\sim C31 \\sim C46 \\sim C33: within 1.7A with sigma
of 0.02 and sigma for terminal atoms of 0.04
4. Others
 Fixed Sof: C1(0.5) C6(0.5) H6(0.5) C0aa(0.5) H0aa(0.5) C4(0.5) H4(0.5)
 C3(0.5) H3(0.5) C5(0.5) H5(0.5) C10(0.5) C8(0.5) H8(0.5) C1aa(0.5) H1aa(0.5)
 C5aa(0.5) H5aa(0.5) C2aa(0.5) H2aa(0.5) C2(0.5) H2(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C29(H29a,H29b), C32(H32a,H32b), C51(H51a,H51b)
5.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C20(H20), C22(H22), C23(H23), C27(H27), C30(H30), C46(H46),
 C31(H31), C4aa(H4aa), C3aa(H3aa), C17(H17), C6(H6), C0aa(H0aa), C4(H4), C3(H3),
  C5(H5), C8(H8), C1aa(H1aa), C5aa(H5aa), C2aa(H2aa), C2(H2)
5.c Fitted hexagon refined as free rotating group:
 C33(C46,C31,C4aa,C3aa,C17), C1(C6,C0aa,C4,C3,C5), C10(C8,C1aa,C5aa,C2aa,C2)
5.d Idealised Me refined as rotating group:
 C28(H28a,H28b,H28c), C44(H44a,H44b,H44c), C56(H56a,H56b,H56c), C68(H68a,H68b,
 H68c)
;