Nuclearity control in calix[4]arene based zinc (II) coordination complexes
KNIAZEVA, Mariia; Ovsyannikov, Alexander; Islamov, Daut; Samigullina, Aida I.; Gubaidullin, Aidar Timergalievich; Dorovatovskii, Pavel; Solovieva, Svetlana; Igor, Antipin S.; Ferlay, Sylvie; CrystEngComm  (2020) –; doi:10.1039/D0CE01232G

data_7241331
_publ_section_title
;
 Nuclearity control in calix[4]arene based zinc (II) coordination
 complexes
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE01232G
_journal_year                    2020
_chemical_formula_moiety         'C94 H84 N2 O18 Zn'
_chemical_formula_sum            'C94 H84 N2 O18 Zn'
_chemical_formula_weight         1595.00
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-04-08
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-07-14 deposited with the CCDC.	2020-09-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   33.388(5)
_cell_length_b                   33.388(5)
_cell_length_c                   22.267(4)
_cell_measurement_reflns_used    500
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      1.3
_cell_volume                     21497(6)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rayonix SX165 CCD'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.79313
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_unetI/netI     0.0301
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            51481
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        28.417
_diffrn_reflns_theta_max         30.973
_diffrn_reflns_theta_min         1.288
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.425
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.109
_exptl_crystal_description       prism
_exptl_crystal_F_000             7524
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.523
_refine_diff_density_min         -1.392
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     525
_refine_ls_number_reflns         10874
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0888
_refine_ls_R_factor_gt           0.0707
_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^)+(0.1371P)^2^+38.5439P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2102
_refine_ls_wR_factor_ref         0.2269
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8131
_reflns_number_total             10874
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01232g1.cif
_cod_data_source_block           mk24s
_cod_original_cell_volume        21497(7)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7241331
_shelx_shelxl_version_number     2018/3
_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, All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C00D(H00A,H00B), C00T(H00C,H00D), C019(H01A,H01B), C01B(H01D,H01E), C01H(H01K,
 H01L), C01I(H01M,H01N)
2.b Aromatic/amide H refined with riding coordinates:
 C00H(H00H), C00J(H00J), C00K(H00K), C00N(H00N), C00O(H00O), C00R(H00R),
 C00X(H00X), C00Y(H00Y), C00Z(H00Z), C011(H011), C013(H013), C015(H015),
 C016(H016), C017(H017), C018(H018), C01A(H01C), C01C(H01F), C01F(H01J),
 C01J(H01O), C01L(H01P), C01M(H01Q)
2.c Idealised Me refined as rotating group:
 C01D(H01G,H01H,H01I), C01N(H01R,H01S,H01T)
2.d Idealised tetrahedral OH refined as rotating group:
 O002(H002), O004(H004), O00E(H00E)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              3489
_shelx_fab_checksum              35717
_olex2_submission_special_instructions 'No special instructions were received'