Oxidation state variation in bis-calix[4]arene supported decametallic Mn clusters
Brechin, Euan K.; Wilson, Lucinda; Coletta, Marco; Jose, Reshma; Rajaraman, Gopalan; Dalgarno, Scott; Dalton Transactions  (2021) –; doi:10.1039/D1DT03410C

data_7708896
_publ_section_title
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 Oxidation state variation in bis-calix[4]arene supported decametallic Mn
 clusters
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03410C
_journal_year                    2021
_chemical_formula_moiety         'C196 H244 Mn10 N6 O32, 2(C2 N)'
_chemical_formula_sum            'C200 H270 Mn10 N8 O32'
_chemical_formula_weight         3847.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-07-26
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-07-26 deposited with the CCDC.	2021-11-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.949(16)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   22.322(6)
_cell_length_b                   18.903(5)
_cell_length_c                   27.501(7)
_cell_measurement_reflns_used    9413
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      68.97
_cell_measurement_theta_min      2.88
_cell_volume                     11100(5)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1384
_diffrn_reflns_av_unetI/netI     0.0760
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            157579
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         73.163
_diffrn_reflns_theta_min         2.253
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.960
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.5505
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1225 before and 0.0810 after correction.
The Ratio of minimum to maximum transmission is 0.7305.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_description       Block
_exptl_crystal_F_000             4064
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.864
_refine_diff_density_min         -1.336
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.403
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     989
_refine_ls_number_reflns         21932
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.405
_refine_ls_R_factor_all          0.1620
_refine_ls_R_factor_gt           0.1271
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3615
_refine_ls_wR_factor_ref         0.3950
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14106
_reflns_number_total             21932
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03410c2.cif
_cod_data_source_block           488
_cod_original_cell_volume        11101(5)
_cod_database_code               7708896
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.588
_shelx_estimated_absorpt_t_min   0.382
_olex2_refinement_description
;
1. Restrained distances
 O11-C102
 1.2 with sigma of 0.02
 O15-C101 = O18-C97
 1.45 with sigma of 0.02
 C9-C10 = C9-C8 = C8-C13 = C12-C11 = C11-C10 = C12-C13
 1.39 with sigma of 0.02
 C82-C81 = C84-C81 = C81-C83 = C77-C78 = C77-C79 = C77-C80
 1.54 with sigma of 0.02
 C43-C41 = C44-C41 = C42-C41
 1.54 with sigma of 0.02
 N5-C98
 1.45 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(C15) = Uanis(C16) = Uanis(C17) = Uanis(C18) = Uanis(C19) = Uanis(C20)
Uanis(C13) = Uanis(C10) = Uanis(C8) = Uanis(C9) = Uanis(C11) = Uanis(C12)
Uanis(C28) = Uanis(C7) = Uanis(C21) = Uanis(C14)
Uanis(O2) = Uanis(O3) = Uanis(O4) = Uanis(O1)
Uanis(N3) = Uanis(N4)
Uanis(N2) = Uanis(N1)
Uanis(C93) = Uanis(C94)
Uanis(C96) = Uanis(C95)
Uanis(C77) = Uanis(C80) = Uanis(C83) = Uanis(C78) = Uanis(C84) = Uanis(C79) =
Uanis(C81) = Uanis(C82)
Uanis(C34) = Uanis(C33) = Uanis(C35) = Uanis(C36)
Uanis(C44) = Uanis(C41) = Uanis(C42) = Uanis(C43)
Uanis(C91) = Uanis(C90) = Uanis(C92) = Uanis(C89)
3. Others
 Fixed Sof: N1(0.45) N2(0.55) N3(0.75) N4(0.25) C81(0.5) C82(0.5) H82A(0.5)
 H82B(0.5) H82C(0.5) C83(0.5) H83A(0.5) H83B(0.5) H83C(0.5) C84(0.5) H84A(0.5)
 H84B(0.5) H84C(0.5) C77(0.5) C78(0.5) H78A(0.5) H78B(0.5) H78C(0.5) C79(0.5)
 H79A(0.5) H79B(0.5) H79C(0.5) C80(0.5) H80A(0.5) H80B(0.5) H80C(0.5)
4.a Ternary CH refined with riding coordinates:
 C28(H28), C72(H72)
4.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C14(H14A,H14B), C21(H21A,H21B), C51(H51A,H51B), C58(H58A,H58B),
 C65(H65A,H65B)
4.c Me refined with riding coordinates:
 C97(H97A,H97B,H97C), C101(H10D,H10E,H10F), C82(H82A,H82B,H82C), C83(H83A,H83B,
 H83C), C84(H84A,H84B,H84C), C78(H78A,H78B,H78C), C79(H79A,H79B,H79C), C80(H80A,
 H80B,H80C)
4.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C9(H9), C11(H11), C16(H16), C18(H18), C23(H23), C25(H25),
 C46(H46), C48(H48), C53(H53), C55(H55), C60(H60), C62(H62), C67(H67), C69(H69),
  C98(H98), C102(H102)
4.e 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), C86(H86A,H86B,H86C), C87(H87A,H87B,H87C), C88(H88A,H88B,H88C), C90(H90A,
 H90B,H90C), C91(H91A,H91B,H91C), C92(H92A,H92B,H92C), C99(H99A,H99B,H99C),
 C100(H10A,H10B,H10C), C103(H10G,H10H,H10I), C104(H10J,H10K,H10L)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              56802
_shelx_hkl_checksum              15011
_shelx_fab_checksum              5544
_olex2_submission_special_instructions 'No special instructions were received'