The Electrochemical Reduction of a Flexible Mn(II) Salen-Based Metal-Organic Framework
Solomon, Marcello B.; Hua, Carol; Chan, Bun; Church, Tamara L.; Cohen, Seth M.; Kubiak, Clifford P.; Jolliffe, Katrina A.; D'Alessandro, Deanna Michelle; Dalton Transactions  (2021) –; doi:10.1039/D1DT02589A

data_7708164
_publ_section_title
;
 The Electrochemical Reduction of a Flexible Mn(II) Salen-Based
 Metal-Organic Framework
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02589A
_journal_year                    2021
_chemical_formula_moiety         'C76 H62 Mn N4 O15 Zn3'
_chemical_formula_sum            'C76 H62 Mn N4 O15 Zn3'
_chemical_formula_weight         1522.34
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-06-24
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2021-01-15 deposited with the CCDC.	2021-08-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.1980(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   65.1518(10)
_cell_length_b                   14.7217(2)
_cell_length_c                   24.4314(4)
_cell_measurement_reflns_used    13507
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      65.7590
_cell_measurement_theta_min      3.7000
_cell_volume                     21992.2(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.15 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.15 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.15 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.5861
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1215
_diffrn_reflns_av_unetI/netI     0.0840
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       81
_diffrn_reflns_limit_h_min       -80
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            141873
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.563
_diffrn_reflns_theta_min         3.770
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.022
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72109
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.15 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    0.920
_exptl_crystal_description       block
_exptl_crystal_F_000             6248
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.749
_refine_diff_density_min         -1.038
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     838
_refine_ls_number_reflns         22242
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.1402
_refine_ls_R_factor_gt           0.0854
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1668P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2385
_refine_ls_wR_factor_ref         0.2798
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11110
_reflns_number_total             22242
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02589a2.cif
_cod_data_source_block           znmntp1bpdc_x
_cod_database_code               7708164
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.888
_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
 O15-Mn2 \\sim Mn2-O14
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C56) = Uanis(C57) = Uanis(C59) = Uanis(C58) = Uanis(N3) = Uanis(N2) =
Uanis(C60) = Uanis(C61) = Uanis(C62) = Uanis(C63) = Uanis(O13) = Uanis(O025) =
Uanis(C73) = Uanis(C72) = Uanis(C71) = Uanis(C70) = Uanis(C69) = Uanis(C68) =
Uanis(C67) = Uanis(C66) = Uanis(C65) = Uanis(C64) = Uanis(C83) = Uanis(C79) =
Uanis(C82) = Uanis(C80) = Uanis(C84) = Uanis(C78) = Uanis(C87) = Uanis(C88) =
Uanis(C86) = Uanis(C81)
Uanis(N4) = Uanis(N5)
Uanis(C57) = Uanis(C56) = Uanis(N4) = Uanis(N5)
Uanis(Mn2) = Uanis(Mn1)
Uanis(C74) = Uanis(C75) = Uanis(C77) = Uanis(C76)
Uanis(O15) = Uanis(O14)
4. Others
 Sof(N5)=Sof(C84)=Sof(C83)=Sof(H83)=Sof(C82)=Sof(H82)=Sof(C81)=Sof(H81)=
 Sof(C88)=Sof(H88)=Sof(C67)=Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(C58)=Sof(H58A)=
 Sof(H58B)=Sof(N2)=Sof(O13)=Sof(C60)=Sof(H60)=Sof(C73)=Sof(C63)=Sof(C65)=
 Sof(H65)=Sof(C69)=Sof(H69)=Sof(C71)=Sof(Mn1)=1-FVAR(1)
 Sof(Mn2)=Sof(O025)=Sof(C68)=Sof(H68)=Sof(C70)=Sof(C64)=Sof(H64)=Sof(N3)=
 Sof(C72)=Sof(C62)=Sof(C61)=Sof(H61)=Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(C57)=
 Sof(H57A)=Sof(H57B)=Sof(N4)=Sof(C78)=Sof(C66)=Sof(C80)=Sof(H80)=Sof(C79)=
 Sof(H79)=Sof(C86)=Sof(H86)=Sof(C87)=Sof(H87)=FVAR(1)
 Fixed Sof: H55A(0.5) H55(0.5) O14(0.5) H14A(0.5) H14B(0.5) O15(0.5) H15A(0.5)
 H15B(0.5)
5.a Rotating group:
 O14(H14A,H14B), O15(H15A,H15B)
5.b Secondary CH2 refined with riding coordinates:
 C56(H56A,H56B), C58(H58A,H58B), C59(H59A,H59B), C57(H57A,H57B)
5.c Aromatic/amide H refined with riding coordinates:
 C20(H20), C00R(H00R), C24(H24), C25(H25), C23(H23), C45(H45), C33(H33),
 C32(H32), C7(H7), C38(H38), C19(H19), C36(H36), C12(H12), C39(H39), C44(H44),
 C17(H17), C16(H16), C3(H3), C22(H22), C10(H10), C35(H35), C51(H51), C6(H6),
 C41(H41), C9(H9), C30(H30), C47(H47), C4(H4), C29(H29), C42(H42), C83(H83),
 C82(H82), C81(H81), C88(H88), C55(H55A), C55(H55), C68(H68), C64(H64),
 C61(H61), C60(H60), C65(H65), C69(H69), C80(H80), C79(H79), C86(H86), C87(H87)
5.d Fitted hexagon refined as free rotating group:
 C84(C83,C82,N1,C81,C88)
5.e Idealised Me refined as rotating group:
 C54(H54A,H54B,H54C), C53(H53A,H53B,H53C), C028(H02A,H02B,H02C), C75(H75A,H75B,
 H75C), C77(H77A,H77B,H77C), C76(H76A,H76B,H76C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              651
_shelx_hkl_checksum              76687
_shelx_fab_checksum              5424
_olex2_submission_special_instructions 'No special instructions were received'