The remarkable influence of N,O-ligands in the assembly of a bis-calix[4]arene-supported [MnMnMn] cluster.
Coletta, Marco; Sanz, Sergio; McCormick, Laura J.; Teat, Simon J.; Brechin, Euan K.; Dalgarno, Scott J.; Dalton transactions (Cambridge, England : 2003)  (2017) –; doi:10.1039/c7dt04233g

data_7044856
_publ_section_title
;
 The remarkable influence of N,O-ligands in the assembly of a
 bis-calix[4]arene-supported [MnMnMn] cluster.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/c7dt04233g
_journal_year                    2017
_chemical_formula_moiety
'C230 H326 Cl6 Mn20 N16 O50, 2(C3 H7 N O), C H3 O2, 2(O)'
_chemical_formula_sum            'C237 H350 Cl6 Mn20 N18 O56'
_chemical_formula_weight         5658.83
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-11-09
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3461 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-11-09 deposited with the CCDC.
2017-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.212(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.3953(7)
_cell_length_b                   45.6912(18)
_cell_length_c                   40.7908(16)
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.07
_cell_measurement_theta_min      2.235
_cell_volume                     33843(2)
_computing_cell_refinement       'SAINT V8.34A Bruker-AXS, Madison WI'
_computing_data_collection       'Bruker APEX3 Bruker-AXS, Madison WI'
_computing_data_reduction        'SAINT V8.34A Bruker-AXS, Madison WI'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       '\w/\q shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0610
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       57
_diffrn_reflns_limit_k_min       -57
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            163555
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         29.119
_diffrn_reflns_theta_min         2.099
_diffrn_source
;
Advanced Light Source, station 11.3.1
;
_exptl_absorpt_coefficient_mu    1.042
_exptl_absorpt_correction_T_max  0.8621
_exptl_absorpt_correction_T_min  0.7805
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0851 before and 0.0627 after correction.
The Ratio of minimum to maximum transmission is 0.9053.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.111
_exptl_crystal_description       Block
_exptl_crystal_F_000             11792
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.521
_refine_diff_density_min         -1.401
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1369
_refine_ls_number_reflns         34860
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1049
_refine_ls_R_factor_gt           0.0822
_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^)+(0.0819P)^2^+402.4733P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2031
_refine_ls_wR_factor_ref         0.2219
_reflns_Friedel_coverage         0.000
_reflns_number_gt                26386
_reflns_number_total             34860
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04233g2.cif
_cod_data_source_block           mc146_d5_a
_cod_database_code               7044856
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.8621
_shelx_estimated_absorpt_t_min   0.7805
_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,H) groups
2. Restrained distances
 N200-C201 = N200-C200 = N200-C202
 1.45 with sigma of 0.02
 O3AA-C202
 1.2 with sigma of 0.02
 O14-C95
 1.2 with sigma of 0.02
 N3-C95 = N3A-C95 = N3-C97 = N3A-C97A = N3-C96 = N3A-C96A
 1.45 with sigma of 0.02
 N2-C100 = N2-C99 = N2-C98
 1.45 with sigma of 0.02
 O11-C98
 1.2 with sigma of 0.02
 N8-C115 = N8-C117 = N8-C116
 1.45 with sigma of 0.02
 O24-C115
 1.2 with sigma of 0.02
 O19-C108
 1.2 with sigma of 0.02
 N6-C108 = N6-C109 = N6-C110
 1.54 with sigma of 0.02
 N1-C90 = N1-C91 = N1-C89
 1.45 with sigma of 0.02
 O10-C89
 1.2 with sigma of 0.02
 C42-C41 = C43-C41 = C41-C44
 1.54 with sigma of 0.02
 C39-C37 = C38-C37 = C40-C37
 1.54 with sigma of 0.02
 C74-C73 = C73-C75 = C73-C76
 1.54 with sigma of 0.02
 C77-C78 = C77-C78A = C77-C80 = C77-C80A = C77-C79 = C77-C79A
 1.54 with sigma of 0.02
 C81-C83 = C81-C82 = C81-C84
 1.54 with sigma of 0.02
 C85-C88 = C87-C85 = C86-C85
 1.54 with sigma of 0.02
 N1-C89 = N1-C89A = N1-C90 = N1-C90A = N1-C91 = N1-C91A
 1.45 with sigma of 0.02
 O10-C89 = O10-C89A
 1.2 with sigma of 0.02
 C202-C200
 2.54 with sigma of 0.04
 C200-C201
 2.54 with sigma of 0.04
 C201-C202
 2.54 with sigma of 0.04
 C95-C97
 2.54 with sigma of 0.04
 C97-C96
 2.54 with sigma of 0.04
 C96-C95
 2.54 with sigma of 0.04
 C95-C97A
 2.54 with sigma of 0.04
 C97A-C96A
 2.54 with sigma of 0.04
 C96A-C95
 2.54 with sigma of 0.04
 C99-C100
 2.54 with sigma of 0.04
 C100-C98
 2.54 with sigma of 0.04
 C98-C99
 2.54 with sigma of 0.04
 C117-C116
 2.54 with sigma of 0.04
 C116-C115
 2.54 with sigma of 0.04
 C115-C117
 2.54 with sigma of 0.04
 C108-C109
 2.54 with sigma of 0.04
 C109-C110
 2.54 with sigma of 0.04
 C110-C108
 2.54 with sigma of 0.04
 C90-C91
 2.54 with sigma of 0.04
 C91-C89
 2.54 with sigma of 0.04
 C89-C90
 2.54 with sigma of 0.04
 C42-C43
 2.54 with sigma of 0.04
 C44-C43
 2.54 with sigma of 0.04
 C44-C42
 2.54 with sigma of 0.04
 C39-C40
 2.54 with sigma of 0.04
 C40-C38
 2.54 with sigma of 0.04
 C38-C39
 2.54 with sigma of 0.04
 C74-C75
 2.54 with sigma of 0.04
 C75-C76
 2.54 with sigma of 0.04
 C76-C74
 2.54 with sigma of 0.04
 C78-C80
 2.54 with sigma of 0.04
 C80-C79
 2.54 with sigma of 0.04
 C79-C78
 2.54 with sigma of 0.04
 C78A-C80A
 2.54 with sigma of 0.04
 C80A-C79A
 2.54 with sigma of 0.04
 C79A-C78A
 2.54 with sigma of 0.04
 C83-C82
 2.54 with sigma of 0.04
 C82-C84
 2.54 with sigma of 0.04
 C84-C83
 2.54 with sigma of 0.04
 C88-C87
 2.54 with sigma of 0.04
 C87-C86
 2.54 with sigma of 0.04
 C86-C88
 2.54 with sigma of 0.04
 C89-C91
 2.54 with sigma of 0.04
 C91-C90
 2.54 with sigma of 0.04
 C90-C89
 2.54 with sigma of 0.04
 C91A-C89A
 2.54 with sigma of 0.04
 C91A-C90A
 2.54 with sigma of 0.04
 C90A-C89A
 2.54 with sigma of 0.04
 C200-C201 \\sim C200-C202
 with sigma of 0.04
 N200-C200 \\sim N200-C201 \\sim N200-C202
 with sigma of 0.02
 N200-C202 \\sim N200-C200
 with sigma of 0.02
 N200-C200 \\sim N200-C201
 with sigma of 0.02
 N200-C201 \\sim N200-C202
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C28) = Uanis(C45A) = Uanis(C45) = Uanis(C28A)
Uanis(N200) = Uanis(C200) = Uanis(C201) = Uanis(C202) = Uanis(O3AA)
Uanis(N3) = Uanis(C96) = Uanis(C97) = Uanis(C97A) = Uanis(N3A) = Uanis(C96A) =
Uanis(C95)
Uanis(C100) = Uanis(N2) = Uanis(C99) = Uanis(C98)
Uanis(C115) = Uanis(N8)
Uanis(C115) = Uanis(C117)
Uanis(C115) = Uanis(C116)
Uanis(C108) = Uanis(N6) = Uanis(C110) = Uanis(C109)
Uanis(C89) = Uanis(N1) = Uanis(C91) = Uanis(C90)
Uanis(C41) = Uanis(C43) = Uanis(C42) = Uanis(C44)
Uanis(C38) = Uanis(C40) = Uanis(C37) = Uanis(C39)
Uanis(C73) = Uanis(C76) = Uanis(C75) = Uanis(C74)
Uanis(C78) = Uanis(C78A) = Uanis(C80) = Uanis(C80A) = Uanis(C79) = Uanis(C79A)
= Uanis(C77)
Uanis(C86) = Uanis(C87) = Uanis(C88) = Uanis(C85)
Uanis(C89) = Uanis(C89A) = Uanis(N1) = Uanis(C91) = Uanis(C91A) = Uanis(C90A) =
Uanis(C90)
Uanis(O200) = Uanis(O201) = Uanis(O202)
Uanis(O201) = Uanis(C203)
4. Others
 Fixed Sof: C28(0.5) H28(0.5) C28A(0.5) H28A(0.5) C45(0.5) H45(0.5) C45A(0.5)
 H45A(0.5) C78(0.75) H78A(0.75) H78B(0.75) H78C(0.75) C78A(0.25) H78D(0.25)
 H78E(0.25) H78F(0.25) C79(0.75) H79A(0.75) H79B(0.75) H79C(0.75) C79A(0.25)
 H79D(0.25) H79E(0.25) H79F(0.25) C80(0.75) H80A(0.75) H80B(0.75) H80C(0.75)
 C80A(0.25) H80D(0.25) H80E(0.25) H80F(0.25) C89(0.6) H89(0.6) C89A(0.4)
 H89A(0.4) C90(0.6) H90D(0.6) H90E(0.6) H90F(0.6) C90A(0.4) H90A(0.4) H90B(0.4)
 H90C(0.4) C91(0.6) H91D(0.6) H91E(0.6) H91F(0.6) C91A(0.4) H91A(0.4) H91B(0.4)
 H91C(0.4) H95(0.6) H95A(0.4) C96(0.6) H96A(0.6) H96B(0.6) H96C(0.6) C96A(0.3)
 H96D(0.3) H96E(0.3) H96F(0.3) C97(0.7) H97A(0.7) H97B(0.7) H97C(0.7) C97A(0.4)
 H97D(0.4) H97E(0.4) H97F(0.4) C203(0.5) H20G(0.5) H20H(0.5) H20I(0.5) N3(0.6)
 N3A(0.4) O200(0.5) O202(0.5)
5.a Rotating group:
 O16(H16A,H16B)
5.b Ternary CH refined with riding coordinates:
 C28(H28), C28A(H28A), C45(H45), C45A(H45A)
5.c Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C14(H14A,H14B), C21(H21A,H21B), C52(H52A,H52B), C59(H59A,H59B),
 C66(H66A,H66B), C101(H10D,H10E), C102(H10F,H10G), C103(H10H,H10I), C104(H10J,
 H10K), C105(H10L,H10M), C106(H10N,H10O), C107(H10P,H10Q), C111(H11P,H11Q),
 C112(H11R,H11S), C113(H11H,H11I), C114(H11A,H11B), C118(H11C,H11D)
5.d Me refined with riding coordinates:
 C78(H78A,H78B,H78C), C78A(H78D,H78E,H78F), C79(H79A,H79B,H79C), C79A(H79D,
 H79E,H79F), C80(H80A,H80B,H80C), C80A(H80D,H80E,H80F), C90(H90D,H90E,H90F),
 C90A(H90A,H90B,H90C), C91(H91D,H91E,H91F), C91A(H91A,H91B,H91C), C96(H96A,H96B,
 H96C), C96A(H96D,H96E,H96F), C97(H97A,H97B,H97C), C97A(H97D,H97E,H97F),
 C99(H99A,H99B,H99C), C100(H10A,H10B,H10C), C116(H11E,H11F,H11G), C117(H11J,
 H11K,H11L)
5.e Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C9(H9), C11(H11), C16(H16), C18(H18), C23(H23), C25(H25),
 C47(H47), C49(H49), C54(H54), C56(H56), C61(H61), C63(H63), C68(H68), C70(H70),
  C89(H89), C89A(H89A), C95(H95), C95(H95A), C98(H98), C108(H108), C115(H115),
 C202(H202)
5.f 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), C38(H38A,H38B,H38C), C39(H39A,
 H39B,H39C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C),
 C44(H44A,H44B,H44C), C74(H74A,H74B,H74C), C75(H75A,H75B,H75C), C76(H76A,H76B,
 H76C), C82(H82A,H82B,H82C), C83(H83A,H83B,H83C), C84(H84A,H84B,H84C), C86(H86A,
 H86B,H86C), C87(H87A,H87B,H87C), C88(H88A,H88B,H88C), C109(H10R,H10S,H10T),
 C110(H11M,H11N,H11O), C200(H20A,H20B,H20C), C201(H20D,H20E,H20F), C203(H20G,
 H20H,H20I)
;
_olex2_submission_special_instructions 'No special instructions were received'