Calix[4]arene-supported trigonal and square prisms of Mn and Na
Wilson, Lucinda R. B.; Dalgarno, Scott J.; Brechin, Euan K.; CrystEngComm 27 (2025) 3041–3047; doi:10.1039/D5CE00285K

data_7250277
_publ_section_title
;
 Calix[4]arene-supported trigonal and square prisms of Mn and Na
;
_journal_issue                   19
_journal_name_full               CrystEngComm
_journal_page_first              3041
_journal_page_last               3047
_journal_paper_doi               10.1039/D5CE00285K
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'C200.2 H256.6 Cl2 Mn6 N8 Na6 O32, 6(C2 H3 N)'
_chemical_formula_sum            'C212.2 H274.6 Cl2 Mn6 N14 Na6 O32'
_chemical_formula_weight         4071.92
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-03-12
_audit_creation_method
;
Olex2 1.5
(compiled 2025.02.27 svn.r83f5de26 for OlexSys, GUI svn.r7181)
;
_audit_update_record
;
2025-03-12 deposited with the CCDC.	2025-04-09 downloaded from the CCDC.
;
_cell_angle_alpha                91.090(2)
_cell_angle_beta                 110.5190(10)
_cell_angle_gamma                109.8950(10)
_cell_formula_units_Z            1
_cell_length_a                   17.5535(4)
_cell_length_b                   18.1099(4)
_cell_length_c                   20.5110(5)
_cell_measurement_reflns_used    9620
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.81
_cell_measurement_theta_min      4.28
_cell_volume                     5670.9(2)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_collection       'Apex 4 (Bruker)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0697
_diffrn_reflns_av_unetI/netI     0.0542
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            223893
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.488
_diffrn_reflns_theta_min         4.276
_diffrn_source_current           1.1
_diffrn_source_power             0.05500000000000001
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.497
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.6216
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0924 before and 0.0688 after correction.
The Ratio of minimum to maximum transmission is 0.8246.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_description       block
_exptl_crystal_F_000             2152
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.608
_refine_diff_density_min         -2.087
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.661
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1405
_refine_ls_number_reflns         23081
_refine_ls_number_restraints     271
_refine_ls_restrained_S_all      1.666
_refine_ls_R_factor_all          0.1387
_refine_ls_R_factor_gt           0.1178
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3792
_refine_ls_wR_factor_ref         0.4061
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16910
_reflns_number_total             23081
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00285k2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7250276--7250277.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C212.20 H274.60 Cl2 Mn6 N14 Na6 O32'
_cod_database_code               7250277
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.640
_shelx_estimated_absorpt_t_min   0.513
_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. Restrained distances
 C88-C86 = C89-C86 = C87-C86
 1.54 with sigma of 0.02
 N2-C102 = N2-C103
 1.45 with sigma of 0.02
 C88A-C86A = C87A-C86A = C89A-C86A = C86A-C67
 1.54 with sigma of 0.02
 C101-C103
 2.4 with sigma of 0.02
 C102-C101
 2.4 with sigma of 0.02
 C102-C103
 2.5 with sigma of 0.02
 C87A-C89A
 2.54 with sigma of 0.04
 C89A-C88A
 2.54 with sigma of 0.04
 C88A-C87A
 2.54 with sigma of 0.04
 C89-C87
 2.54 with sigma of 0.04
 C87-C88
 2.54 with sigma of 0.04
 C88-C89
 2.54 with sigma of 0.04
 C67-C86 \\sim C67-C86A
 with sigma of 0.02
 C86-C87 \\sim C86A-C87A
 with sigma of 0.02
 C86-C88 \\sim C86A-C88A
 with sigma of 0.02
 C86-C89 \\sim C86A-C89A
 with sigma of 0.02
 C67-C87 \\sim C67-C87A
 with sigma of 0.04
 C67-C88 \\sim C67-C88A
 with sigma of 0.04
 C67-C89 \\sim C67-C89A
 with sigma of 0.04
 C87-C88 \\sim C87A-C88A
 with sigma of 0.04
 C87-C89 \\sim C87A-C89A
 with sigma of 0.04
 C88-C89 \\sim C88A-C89A
 with sigma of 0.04
3. Rigid body (RIGU) restrains
 C38, C39, C41, C43, C40, C42, C44
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C90, C91, C93, C95, C92, C94, C96
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 N3, C105, C106, C107, O17
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O18, N4, C108, C109, C110
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O15, O16, C104
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O14, N2, C101, C102, C103
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O19, N1, C98, C99, C100
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O12, C117, O9, O10, C97, O11, O13
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C86, C87, C88, C89, C86A, C89A, C87A, C88A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Fixed Sof: C86(0.8) C87(0.8) H87A(0.8) H87B(0.8) H87C(0.8) C88(0.8) H88A(0.8)
 H88B(0.8) H88C(0.8) C89(0.8) H89A(0.8) H89B(0.8) H89C(0.8) C101(0.5) H101(0.5)
 C102(0.5) H10D(0.5) H10E(0.5) H10F(0.5) C103(0.5) H10G(0.5) H10H(0.5)
 H10I(0.5) O9(0.4) O13(0.4) O16(0.4) C29(0.333333) H29(0.333333) C39(0.5)
 H39A(0.5) H39B(0.5) H39C(0.5) C41(0.5) H41A(0.5) H41B(0.5) H41C(0.5) C43(0.5)
 H43A(0.5) H43B(0.5) H43C(0.5) C49(0.333333) H49(0.333333) C91(0.5) H91A(0.5)
 H91B(0.5) H91C(0.5) C93(0.5) H93A(0.5) H93B(0.5) H93C(0.5) C95(0.5) H95A(0.5)
 H95B(0.5) H95C(0.5) O10(0.6) O11(0.6) O15(0.6) C28(0.6667) H28(0.6667)
 C40(0.5) H40A(0.5) H40B(0.5) H40C(0.5) C42(0.5) H42A(0.5) H42B(0.5) H42C(0.5)
 C44(0.5) H44A(0.5) H44B(0.5) H44C(0.5) C50(0.6667) H50(0.6667) C92(0.5)
 H92A(0.5) H92B(0.5) H92C(0.5) C94(0.5) H94A(0.5) H94B(0.5) H94C(0.5) C96(0.5)
 H96A(0.5) H96B(0.5) H96C(0.5) C97(0.6) C104(0.6) H10S(0.6) H10T(0.6) H10U(0.6)
 C117(0.4) C86A(0.2) C89A(0.2) H89D(0.2) H89E(0.2) H89F(0.2) C87A(0.2)
 H87D(0.2) H87E(0.2) H87F(0.2) C88A(0.2) H88D(0.2) H88E(0.2) H88F(0.2)
5.a Ternary CH refined with riding coordinates:
 C29(H29), C49(H49), C28(H28), C50(H50)
5.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C14(H14A,H14B), C21(H21A,H21B), C57(H57A,H57B), C64(H64A,H64B),
 C71(H71A,H71B)
5.c Me refined with riding coordinates:
 C87(H87A,H87B,H87C), C88(H88A,H88B,H88C), C89(H89A,H89B,H89C), C99(H99A,H99B,
 H99C), C100(H10A,H10B,H10C), C102(H10D,H10E,H10F), C103(H10G,H10H,H10I),
 C106(H10J,H10K,H10L), C107(H10M,H10N,H10O), C109(H10P,H10Q,H10R), C110(H11A,
 H11B,H11C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C),
 C91(H91A,H91B,H91C), C93(H93A,H93B,H93C), C95(H95A,H95B,H95C), C40(H40A,H40B,
 H40C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C92(H92A,H92B,H92C), C94(H94A,
 H94B,H94C), C96(H96A,H96B,H96C), C104(H10S,H10T,H10U), C89A(H89D,H89E,H89F),
 C87A(H87D,H87E,H87F), C88A(H88D,H88E,H88F)
5.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C9(H9), C11(H11), C16(H16), C18(H18), C23(H23), C25(H25),
 C52(H52), C54(H54), C59(H59), C61(H61), C66(H66), C68(H68), C73(H73), C75(H75),
  C98(H98), C101(H101), C105(H105), C108(H108)
5.e Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C35(H35A,H35B,
 H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C46(H46A,H46B,H46C), C47(H47A,
 H47B,H47C), C48(H48A,H48B,H48C), C79(H79A,H79B,H79C), C80(H80A,H80B,H80C),
 C81(H81A,H81B,H81C), C83(H83A,H83B,H83C), C84(H84A,H84B,H84C), C85(H85A,H85B,
 H85C), C111(H11D,H11E,H11F), C113(H11G,H11H,H11I), C115(H11J,H11K,H11L)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              34029
_shelx_fab_checksum              76679
_olex2_submission_special_instructions 'No special instructions were received'