Passing it up the ranks: hierarchical ion-size dependent supramolecular response in 1D coordination polymers
Sensharma, Debobroto; Wix, Paul; Kathalikkattil, Amal Cherian; Schmitt, Wolfgang; CrystEngComm 20 (2018) 5127–; doi:10.1039/C8CE01211C

data_7231398
_publ_section_title
;
 Passing it up the ranks: hierarchical ion-size dependent supramolecular
 response in 1D coordination polymers
;
_journal_issue                   35
_journal_name_full               CrystEngComm
_journal_page_first              5127
_journal_paper_doi               10.1039/C8CE01211C
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C45 H28 Mn N6 O6, 1.25(C3 H7 N O)'
_chemical_formula_sum            'C48.75 H36.75 Mn N7.25 O7.25'
_chemical_formula_weight         895.04
_chemical_name_systematic
'catena-[(2,4,6-tri(pyridin-2-yl)-1,3,5-triazine)-(\m~5~-hydrogen benzene-1,3,5-tris(4-benzoato))]-manganese(II)-N,N'-dimethylformamide solvate]'
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-06-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-06-28 deposited with the CCDC.
2018-08-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.280(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.2604(6)
_cell_length_b                   17.3810(6)
_cell_length_c                   30.3417(10)
_cell_measurement_reflns_used    9884
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.42
_cell_measurement_theta_min      3.65
_cell_volume                     8409.6(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      99.99
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_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  0.0460
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            58048
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.473
_diffrn_reflns_theta_min         2.542
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.088
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6538
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0689 before and 0.0555 after correction. The Ratio of minimum to maximum transmission is 0.8681. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_description       block
_exptl_crystal_F_000             3704
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.847
_refine_diff_density_min         -0.723
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1334
_refine_ls_number_reflns         15442
_refine_ls_number_restraints     424
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0636
_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^)+(0.0986P)^2^+8.2832P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1723
_refine_ls_wR_factor_ref         0.1847
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12369
_reflns_number_total             15442
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01211c2.cif
_cod_data_source_block           pw084
_cod_depositor_comments
'Adding full bibliography for 7231397--7231400.cif.'
_cod_database_code               7231398
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.790
_shelx_estimated_absorpt_t_min   0.638
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 N13_1-C93_1
 N13_2-C93_2
 N13_3-C93_3
 N13_4-C93_4
 N13_5-C93_5
 N13_6-C93_6
 1.3625 with sigma of 0.02
 N13_1-C95_1
 N13_2-C95_2
 N13_3-C95_3
 N13_4-C95_4
 N13_5-C95_5
 N13_6-C95_6
 1.4533 with sigma of 0.02
 N13_1-C94_1
 N13_2-C94_2
 N13_3-C94_3
 N13_4-C94_4
 N13_5-C94_5
 N13_6-C94_6
 1.4503 with sigma of 0.02
 O13_1-C93_1
 O13_2-C93_2
 O13_3-C93_3
 O13_4-C93_4
 O13_5-C93_5
 O13_6-C93_6
 1.2164 with sigma of 0.02
 O12-C85 = O11-C85
 1.26 with sigma of 0.01
 O7-O13_4
 3 with sigma of 0.02
 C93_1-C95_1
 C93_2-C95_2
 C93_3-C95_3
 C93_4-C95_4
 C93_5-C95_5
 C93_6-C95_6
 2.4456 with sigma of 0.01
 C95_1-C94_1
 C95_2-C94_2
 C95_3-C94_3
 C95_4-C94_4
 C95_5-C94_5
 C95_6-C94_6
 2.4848 with sigma of 0.01
 C94_1-C93_1
 C94_2-C93_2
 C94_3-C93_3
 C94_4-C93_4
 C94_5-C93_5
 C94_6-C93_6
 2.4578 with sigma of 0.01
 O13_1-N13_1
 O13_2-N13_2
 O13_3-N13_3
 O13_4-N13_4
 O13_5-N13_5
 O13_6-N13_6
 2.2984 with sigma of 0.01
 O13_1-C95_1
 O13_2-C95_2
 O13_3-C95_3
 O13_4-C95_4
 O13_5-C95_5
 O13_6-C95_6
 2.828 with sigma of 0.04
 C79A-C75 \\sim C79-C75
 with sigma of 0.02
3. Restrained planarity
 C95_1, C94_1, N13_1, C93_1, O13_1
 C95_2, C94_2, N13_2, C93_2, O13_2
 C95_3, C94_3, N13_3, C93_3, O13_3
 C95_4, C94_4, N13_4, C93_4, O13_4
 C95_5, C94_5, N13_5, C93_5, O13_5
 C95_6, C94_6, N13_6, C93_6, O13_6
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
H94C_4 \\sim H95C_4: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08
C79A \\sim C80A \\sim C81A \\sim C82A \\sim C83A \\sim C84A \\sim C85A \\sim
O11A \\sim O12A \\sim C79 \\sim C80 \\sim C81 \\sim C82 \\sim C83 \\sim C84
\\sim C85 \\sim O12 \\sim O11: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C95_5) = Uanis(C93_1) = Uanis(C94_6) = Uanis(C94_5) = Uanis(C95_1) =
Uanis(C95_6) = Uanis(C93_5) = Uanis(C94_1) = Uanis(C93_6)
Uanis(N13_6) = Uanis(N13_5) = Uanis(N13_1)
Uanis(O13_1) = Uanis(O13_6) = Uanis(O13_5)
5. Same fragment restrains
{C95_2, C94_2, N13_2, C93_2, O13_2}
{C95_3, C94_3, N13_3, C93_3, O13_3}
{C95_4, C94_4, N13_4, C93_4, O13_4}
{C95_5, C94_5, N13_5, C93_5, O13_5}
{C95_6, C94_6, N13_6, C93_6, O13_6}
as
{C95_1, C94_1, N13_1, C93_1, O13_1} sigma for 1-2: 0.02 1-3: 0.04
6. Others
 Fixed Sof: C79A(0.5) C80A(0.5) H80A(0.5) C81A(0.5) H81A(0.5) C82A(0.5)
 C83A(0.5) H83A(0.5) C84A(0.5) H84A(0.5) C85A(0.5) O11A(0.5) O12A(0.5) C79(0.5)
 C80(0.5) H80(0.5) C81(0.5) H81(0.5) C82(0.5) C83(0.5) H83(0.5) C84(0.5)
 H84(0.5) C85(0.5) O12(0.5) O11(0.5) C95(0.5) H95A(0.5) H95B(0.5) H95C(0.5)
 C94(0.5) H94A(0.5) H94B(0.5) H94C(0.5) N13(0.5) C93(0.5) H93(0.5) O13(0.5)
 C95(0.5) H95A(0.5) H95B(0.5) H95C(0.5) C94(0.5) H94A(0.5) H94B(0.5) H94C(0.5)
 N13(0.5) C93(0.5) H93(0.5) O13(0.5) C95(0.5) H95A(0.5) H95B(0.5) H95C(0.5)
 C94(0.5) H94A(0.5) H94B(0.5) H94C(0.5) N13(0.5) C93(0.5) H93(0.5) O13(0.5)
 C95(0.5) H95A(0.5) H95B(0.5) H95C(0.5) C94(0.5) H94A(0.5) H94B(0.5) H94C(0.5)
 C93(0.5) H93(0.5) O13(0.5) C95(0.25) H95A(0.25) H95B(0.25) H95C(0.25)
 C94(0.25) H94A(0.25) H94B(0.25) H94C(0.25) N13(0.25) C93(0.25) H93(0.25)
 O13(0.25) C95(0.25) H95A(0.25) H95B(0.25) H95C(0.25) C94(0.25) H94A(0.25)
 H94B(0.25) H94C(0.25) N13(0.25) C93(0.25) H93(0.25) O13(0.25)
7.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C10(H10A), C11(H11), C0AA(H0AA), C13(H13),
 C15(H15), C16(H16), C17(H17), C18(H18), C41(H41), C42(H42), C44(H44), C45(H45),
  C47(H47), C49(H49), C51(H51), C53(H53), C54(H54), C56(H56), C57(H57),
 C60(H60), C61(H61), C63(H63), C64(H64), C20(H20), C21(H21), C22(H22), C23(H23),
  C29(H29), C30(H30), C31(H31), C32(H32), C37(H37), C36(H36), C35(H35),
 C34(H34), C68(H68), C69(H69), C71(H71), C72(H72), C74(H74), C76(H76), C78(H78),
  C80A(H80A), C81A(H81A), C83A(H83A), C84A(H84A), C87(H87), C88(H88), C90(H90),
 C91(H91), C80(H80), C81(H81), C83(H83), C84(H84), C93(H93), C93(H93), C93(H93),
  C93(H93), C93(H93), C93(H93)
7.b Idealised Me refined as rotating group:
 C95(H95A,H95B,H95C), C94(H94A,H94B,H94C), C95(H95A,H95B,H95C), C94(H94A,H94B,
 H94C), C95(H95A,H95B,H95C), C94(H94A,H94B,H94C), C95(H95A,H95B,H95C), C94(H94A,
 H94B,H94C), C95(H95A,H95B,H95C), C94(H94A,H94B,H94C), C95(H95A,H95B,H95C),
 C94(H94A,H94B,H94C)
7.c Idealised tetrahedral OH refined as rotating group:
 O4(H4A), O10(H10)
;
_shelx_res_checksum              19378
_olex2_submission_special_instructions 'No special instructions were received'