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_7250276
_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
'2(C147 H198 Cl Mn3 Na6 O22 S7), 10(C2 H3 N), 2[CH3CN]'
_chemical_formula_sum            'C318 H432 Cl2 Mn6 N12 Na12 O44 S14'
_chemical_formula_weight         6251.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 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                90
_cell_angle_beta                 100.104(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   34.6511(7)
_cell_length_b                   20.6506(5)
_cell_length_c                   24.2274(6)
_cell_measurement_reflns_used    9939
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.48
_cell_measurement_theta_min      2.97
_cell_volume                     17067.4(7)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.980
_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_unetI/netI     0.0903
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_number            16571
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.511
_diffrn_reflns_theta_min         2.974
_diffrn_source_current           1.1
_diffrn_source_power             0.05500000000000001
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.371
_exptl_absorpt_correction_T_max  0.753578
_exptl_absorpt_correction_T_min  0.473794
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1042 before and 0.0688 after correction.
 
For component 2:
 wR2(int) was 0.1211 before and 0.0763 after correction.
 The Ratio of minimum to maximum transmission is 0.63.

Final HKLF 4 output contains 137474 reflections, Rint = 0.0841
 (41283 with I > 3sig(I), Rint = 0.0564)
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_description       block
_exptl_crystal_F_000             6632
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.949
_refine_diff_density_min         -0.904
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1006
_refine_ls_number_reflns         16571
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1326
_refine_ls_R_factor_gt           0.1094
_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^)+(0.1125P)^2^+171.0843P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2704
_refine_ls_wR_factor_ref         0.2844
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13077
_reflns_number_total             16571
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00285k2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7250276--7250277.cif.'
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7250276
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.552
_shelx_estimated_absorpt_t_min   0.431
_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 C(H,H,H,H,H,H) groups
2. Restrained distances
 C41-C37 = C40-C37 = C39-C37 = C38-C37 = C43-C37 = C42-C37
 1.54 with sigma of 0.02
 S5-C78 = S5-C77 = S4-C77 = S4-C78
 1.8 with sigma of 0.02
 C80-C79
 1.45 with sigma of 0.02
 N1-C80
 1.15 with sigma of 0.02
 C39-C41
 2.54 with sigma of 0.02
 C41-C43
 2.54 with sigma of 0.02
 C43-C39
 2.54 with sigma of 0.02
 C40-C42
 2.54 with sigma of 0.02
 C42-C38
 2.54 with sigma of 0.02
 C38-C40
 2.54 with sigma of 0.02
 C37-C38 \\sim C37-C43
 with sigma of 0.02
 C37-C40 \\sim C37-C39
 with sigma of 0.02
 C37-C42 \\sim C37-C41
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 S1, O10, C71, C72
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 S3, O12, C75, C76
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C37, C38, C40, C42, C39, C41, C43
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C79, C80, N1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Fixed Sof: H77A(0.75) H77B(0.75) H77C(0.75) H77D(0.25) H77E(0.25) H77F(0.25)
 H78A(0.75) H78B(0.75) H78C(0.75) H78D(0.25) H78E(0.25) H78F(0.25) S4(0.75)
 C38(0.6) H38A(0.6) H38B(0.6) H38C(0.6) C40(0.6) H40A(0.6) H40B(0.6) H40C(0.6)
 C42(0.6) H42A(0.6) H42B(0.6) H42C(0.6) Cl1(0.5) S5(0.25) O8(0.5) C39(0.4)
 H39A(0.4) H39B(0.4) H39C(0.4) C41(0.4) H41A(0.4) H41B(0.4) H41C(0.4) C43(0.4)
 H43A(0.4) H43B(0.4) H43C(0.4) S2(0.5) O7(0.5) O9(0.5) O11(0.5) C73(0.5)
 H73A(0.5) H73B(0.5) H73C(0.5) C74(0.5) H74A(0.5) H74B(0.5) H74C(0.5) H81A(0.5)
 H81B(0.5) H81C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C14(H14A,H14B), C21(H21A,H21B), C28(H28A,H28B), C48(H48A,H48B),
 C55(H55A,H55B)
5.b Me refined with riding coordinates:
 C38(H38A,H38B,H38C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C39(H39A,H39B,
 H39C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C9(H9), C11(H11), C16(H16), C18(H18), C23(H23), C25(H25),
 C50(H50), C52(H52), C57(H57), C59(H59)
5.d Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C34(H34A,H34B,
 H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C45(H45A,H45B,H45C), C46(H46A,
 H46B,H46C), C47(H47A,H47B,H47C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C),
 C65(H65A,H65B,H65C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C69(H69A,H69B,
 H69C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C75(H75A,H75B,H75C), C76(H76A,
 H76B,H76C), C77(H77A,H77B,H77C), C77(H77D,H77E,H77F), C78(H78A,H78B,H78C),
 C78(H78D,H78E,H78F), C73(H73A,H73B,H73C), C74(H74A,H74B,H74C), C79(H79A,H79B,
 H79C), C81(H81A,H81B,H81C), C83(H83A,H83B,H83C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              11233
_shelx_fab_checksum              36840
_olex2_submission_special_instructions 'No special instructions were received'