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_1566014
_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         'C76 H72 N8 O8 Zn2'
_chemical_formula_sum            'C76 H72 N8 O8 Zn2'
_chemical_formula_weight         1356.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 96.318(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.6846(7)
_cell_length_b                   14.7454(5)
_cell_length_c                   20.9637(7)
_cell_measurement_reflns_used    9760
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      24.102
_cell_measurement_theta_min      2.341
_cell_volume                     6662.4(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.9990
_diffrn_measured_fraction_theta_max 0.9990
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            151840
_diffrn_reflns_theta_full        25.7271
_diffrn_reflns_theta_max         25.73
_diffrn_reflns_theta_min         0.94
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.784
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6932
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.3520
_exptl_crystal_description       block
_exptl_crystal_F_000             2835.5921
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.5681
_refine_diff_density_min         -0.5078
_refine_diff_density_rms         0.0893
_refine_ls_d_res_high            0.8187
_refine_ls_d_res_low             21.5529
_refine_ls_goodness_of_fit_ref   1.1202
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    120
_refine_ls_number_parameters     855
_refine_ls_number_reflns         12681
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.1202
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0397
_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^)+(0.0480P)^2^+6.9884P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0912
_refine_ls_wR_factor_ref         0.1070
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              26
_reflns_limit_h_min              -26
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                10668
_reflns_number_total             12681
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ICA-2022-529-120653.cif
_cod_data_source_block           Zn2X2
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1566014
_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.a Secondary CH2 refined with riding coordinates:
 C14(H14a,H14b), C7(H7a,H7b), C32(H32a,H32b), C28(H28a,H28b), C52(H52a,H52b),
 C45(H45a,H45b), C66(H66a,H66b), C70(H70a,H70b)
2.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C5(H5), C4(H4), C3(H3), C2(H2), C1(H1), C23(H23), C38(H38),
 C37(H37), C36(H36), C35(H35), C34(H34), C54(H54), C39(H39), C40(H40), C41(H41),
  C42(H42), C43(H43), C56(H56), C57(H57), C58(H58), C59(H59), C61(H61),
 C76(H76), C75(H75), C74(H74), C73(H73), C72(H72), C21(H21), C20(H20), C19(H19),
  C18(H18)
2.c Idealised Me refined as rotating group:
 C15(H15a,H15b,H15c), C13(H13a,H13b,H13c), C30(H30a,H30b,H30c), C29(H29a,H29b,
 H29c), C53(H53a,H53b,H53c), C51(H51a,H51b,H51c), C68(H68a,H68b,H68c), C67(H67a,
 H67b,H67c)
;