A Brucite-Like Mixed-Valent Cluster Capped by [MnIIIp-tBu-calix[4]arene]− Moieties
Coletta, Marco; Palacios, Maria A.; Brechin, Euan K.; Dalgarno, Scott J.; Chemistry 2 (2020) 253–261; doi:10.3390/chemistry2020016

data_1558001
_publ_section_title
;
 A Brucite-Like Mixed-Valent Cluster Capped by
 [MnIIIp-tBu-calix[4]arene]&#x2212; Moieties
;
_journal_issue                   2
_journal_name_full               Chemistry
_journal_page_first              253
_journal_page_last               261
_journal_paper_doi               10.3390/chemistry2020016
_journal_volume                  2
_journal_year                    2020
_chemical_formula_moiety         'C200 H264 Cl2 Mn12 N8 O40, 2(C2 H3 N)'
_chemical_formula_sum            'C204 H288 Cl2 Mn12 N10 O40'
_chemical_formula_weight         4250.61
_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     direct
_audit_creation_date             2020-03-26
_audit_creation_method
;
Olex2 1.3
(compiled 2020.01.31 svn.r88ba2a32 for OlexSys, GUI svn.r6032)
;
_cell_angle_alpha                110.119(15)
_cell_angle_beta                 104.06(2)
_cell_angle_gamma                90.752(15)
_cell_formula_units_Z            1
_cell_length_a                   16.144(16)
_cell_length_b                   19.437(19)
_cell_length_c                   22.33(2)
_cell_measurement_reflns_used    2634
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.48
_cell_measurement_theta_min      1.735
_cell_volume                     6346(11)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'Apex II'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-1997  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker X8 Apex II CCD Diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            98657
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.671
_exptl_absorpt_coefficient_mu    0.656
_exptl_absorpt_correction_T_max  0.843
_exptl_absorpt_correction_T_min  0.815
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Bruker-SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.112
_exptl_crystal_description       block
_exptl_crystal_F_000             2236
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.835
_refine_diff_density_min         -1.452
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1188
_refine_ls_number_reflns         25871
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0564
_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^)+(0.1183P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1696
_refine_ls_wR_factor_ref         0.1810
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19129
_reflns_number_total             25871
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            chemistry-773453-supplementary.cif
_cod_data_source_block           Mn12
_cod_depositor_comments          'Adding full bibliography for 1558001.cif.'
_cod_original_cell_volume        6347(11)
_cod_database_code               1558001
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.828
_shelx_estimated_absorpt_t_min   0.779
_exptl_absorpt_special_details
;
 Data were corrected for decay and absorption using the program SADABS
 based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995).
;
_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. Shared sites
{C120, C12A}
3. Restrained distances
 C121-C120
 1.45 with sigma of 0.02
 C12B-C12A
 1.45 with sigma of 0.02
 C121-N4
 1.15 with sigma of 0.02
 C12B-N4A
 1.15 with sigma of 0.02
 C71-C94
 1.54 with sigma of 0.02
 C71-C94A
 1.54 with sigma of 0.02
 C94-C98
 1.54 with sigma of 0.02
 C94-C100
 1.54 with sigma of 0.02
 C94-C96
 1.54 with sigma of 0.02
 C95-C94A
 1.54 with sigma of 0.02
 C99-C94A
 1.54 with sigma of 0.02
 C97-C94A
 1.54 with sigma of 0.02
 C76-C82
 1.54 with sigma of 0.02
 C76-C80
 1.54 with sigma of 0.02
 C76-C78
 1.54 with sigma of 0.02
 C76-C77
 1.54 with sigma of 0.02
 C76-C81
 1.54 with sigma of 0.02
 C76-C79
 1.54 with sigma of 0.02
 C87-C91
 1.54 with sigma of 0.02
 C87-C93
 1.54 with sigma of 0.02
 C87-C89
 1.54 with sigma of 0.02
 C87-C92
 1.54 with sigma of 0.02
 C87-C90
 1.54 with sigma of 0.02
 C87-C88
 1.54 with sigma of 0.02
 C34-C36
 2.54 with sigma of 0.02
 C38-C36
 2.54 with sigma of 0.02
 C34-C38
 2.54 with sigma of 0.02
 C35-C37
 2.54 with sigma of 0.02
 C39-C37
 2.54 with sigma of 0.02
 C35-C39
 2.54 with sigma of 0.02
 C77-C79
 2.54 with sigma of 0.02
 C81-C79
 2.54 with sigma of 0.02
 C77-C81
 2.54 with sigma of 0.02
 C78-C80
 2.54 with sigma of 0.02
 C82-C80
 2.54 with sigma of 0.02
 C78-C82
 2.54 with sigma of 0.02
 C88-C90
 2.54 with sigma of 0.02
 C92-C90
 2.54 with sigma of 0.02
 C88-C92
 2.54 with sigma of 0.02
 C89-C91
 2.54 with sigma of 0.02
 C93-C91
 2.54 with sigma of 0.02
 C89-C93
 2.54 with sigma of 0.02
 C95-C97
 2.54 with sigma of 0.02
 C99-C97
 2.54 with sigma of 0.02
 C95-C99
 2.54 with sigma of 0.02
 C96-C98
 2.54 with sigma of 0.02
 C100-C98
 2.54 with sigma of 0.02
 C96-C100
 2.54 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C33) = Uanis(C34) = Uanis(C35) = Uanis(C36) = Uanis(C37) = Uanis(C38) =
Uanis(C39)
Uanis(C76) = Uanis(C77) = Uanis(C78) = Uanis(C79) = Uanis(C80) = Uanis(C81) =
Uanis(C82)
Uanis(C87) = Uanis(C88) = Uanis(C89) = Uanis(C90) = Uanis(C91) = Uanis(C92) =
Uanis(C93)
Uanis(C94) = Uanis(C94A) = Uanis(C95) = Uanis(C96) = Uanis(C97) = Uanis(C98) =
Uanis(C99) = Uanis(C100)
Uanis(C120) = Uanis(C12A) = Uanis(C121) = Uanis(C12B) = Uanis(N4) = Uanis(N4A)
5. Others
 Fixed Sof: C35(0.5) H35A(0.5) H35B(0.5) H35C(0.5) C37(0.5) H37A(0.5)
 H37B(0.5) H37C(0.5) C39(0.5) H39A(0.5) H39B(0.5) H39C(0.5) C78(0.5) H78A(0.5)
 H78B(0.5) H78C(0.5) C80(0.5) H80A(0.5) H80B(0.5) H80C(0.5) C82(0.5) H82A(0.5)
 H82B(0.5) H82C(0.5) C89(0.5) H89A(0.5) H89B(0.5) H89C(0.5) C91(0.5) H91A(0.5)
 H91B(0.5) H91C(0.5) C93(0.5) H93A(0.5) H93B(0.5) H93C(0.5) C94(0.75) C96(0.75)
 H96A(0.75) H96B(0.75) H96C(0.75) C98(0.75) H98A(0.75) H98B(0.75) H98C(0.75)
 C100(0.75) H10A(0.75) H10B(0.75) H10C(0.75) C34(0.5) H34A(0.5) H34B(0.5)
 H34C(0.5) C36(0.5) H36A(0.5) H36B(0.5) H36C(0.5) C38(0.5) H38A(0.5) H38B(0.5)
 H38C(0.5) C77(0.5) H77A(0.5) H77B(0.5) H77C(0.5) C79(0.5) H79A(0.5) H79B(0.5)
 H79C(0.5) C81(0.5) H81A(0.5) H81B(0.5) H81C(0.5) C88(0.5) H88A(0.5) H88B(0.5)
 H88C(0.5) C90(0.5) H90A(0.5) H90B(0.5) H90C(0.5) C92(0.5) H92A(0.5) H92B(0.5)
 H92C(0.5) C94A(0.25) C95(0.25) H95A(0.25) H95B(0.25) H95C(0.25) C97(0.25)
 H97A(0.25) H97B(0.25) H97C(0.25) C99(0.25) H99A(0.25) H99B(0.25) H99C(0.25)
 N4(0.75) C120(0.75) H12G(0.75) H12H(0.75) H12I(0.75) C121(0.75) N4A(0.25)
 C12A(0.25) H12J(0.25) H12K(0.25) H12L(0.25) C12B(0.25)
6.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C14(H14A,H14B), C21(H21A,H21B), C28(H28A,H28B), C54(H54A,H54B),
 C61(H61A,H61B), C68(H68A,H68B), C75(H75A,H75B)
6.b Me refined with riding coordinates:
 C35(H35A,H35B,H35C), C37(H37A,H37B,H37C), C39(H39A,H39B,H39C), C78(H78A,H78B,
 H78C), C80(H80A,H80B,H80C), C82(H82A,H82B,H82C), C89(H89A,H89B,H89C), C91(H91A,
 H91B,H91C), C93(H93A,H93B,H93C), C96(H96A,H96B,H96C), C98(H98A,H98B,H98C),
 C100(H10A,H10B,H10C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C38(H38A,H38B,
 H38C), C77(H77A,H77B,H77C), C79(H79A,H79B,H79C), C81(H81A,H81B,H81C), C88(H88A,
 H88B,H88C), C90(H90A,H90B,H90C), C92(H92A,H92B,H92C), C95(H95A,H95B,H95C),
 C97(H97A,H97B,H97C), C99(H99A,H99B,H99C), C123(H12A,H12B,H12C), C124(H12D,H12E,
 H12F)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C9(H9), C11(H11), C16(H16), C18(H18), C23(H23), C25(H25),
 C49(H49), C51(H51), C56(H56), C58(H58), C63(H63), C65(H65), C70(H70), C72(H72),
  C110(H110), C113(H113), C116(H116), C122(H122)
6.d Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C41(H41A,H41B,
 H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C45(H45A,H45B,H45C), C46(H46A,
 H46B,H46C), C47(H47A,H47B,H47C), C84(H84A,H84B,H84C), C85(H85A,H85B,H85C),
 C86(H86A,H86B,H86C), C111(H11A,H11B,H11C), C112(H11D,H11E,H11F), C114(H11G,
 H11H,H11I), C115(H11J,H11K,H11L), C117(H11M,H11N,H11O), C118(H11P,H11Q,H11R),
 C120(H12G,H12H,H12I), C12A(H12J,H12K,H12L)
;
_shelx_res_checksum              13970
_shelx_hkl_checksum              36676
_olex2_submission_special_instructions 'No special instructions were received'