Synthesis and magnetic properties of Two Mn-based coordination polymers constructed by mixed-ligand strategy
Zhang, Yujuan; Gao, Lingling; Zhou, Wendi; Wei, Xiao-Qin; Hu, Tuoping; CrystEngComm  (2020) –; doi:10.1039/D0CE01178A

data_7241282
_publ_section_title
;
 Synthesis and magnetic properties of Two Mn-based coordination polymers
 constructed by mixed-ligand strategy
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE01178A
_journal_year                    2020
_chemical_formula_moiety         'C29 H26 Mn2 N2 O13, H2 O'
_chemical_formula_sum            'C29 H28 Mn2 N2 O14'
_chemical_formula_weight         738.41
_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   mixed
_audit_creation_date             2018-02-07
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.02.02 svn.r3481 for OlexSys, GUI svn.r5467)
;
_audit_update_record
;
2019-12-24 deposited with the CCDC.	2020-09-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.908(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2419(7)
_cell_length_b                   15.4637(7)
_cell_length_c                   18.8598(9)
_cell_measurement_reflns_used    6535
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      22.528
_cell_measurement_theta_min      3.091
_cell_volume                     3674.8(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71076
_diffrn_reflns_av_R_equivalents  0.1683
_diffrn_reflns_av_unetI/netI     0.1340
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            54100
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.243
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         3.290
_exptl_absorpt_coefficient_mu    0.749
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6745
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0830 before and 0.0735 after correction. The Ratio of minimum to maximum transmission is 0.9046. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_description       block
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.293
_exptl_crystal_size_mid          0.234
_exptl_crystal_size_min          0.051
_platon_squeeze_details
;
TITL huj4_0m   P 1 21/n 1   R = 0.09
CELL   13.2419   15.4637   18.8598     90.00    107.91     90.00
SPGR P21/n
C101 0.046 0.643 0.955 !       2.18 eA-3
C102 0.969 0.456 0.065 !       2.05 eA-3
C103 1.001 0.657 0.933 !       2.03 eA-3
C104 0.483 0.099 0.577 !       1.99 eA-3
C105 0.424 0.817 0.426 !       1.99 eA-3
C106 0.894 0.598 0.751 !       1.95 eA-3
C107 0.452 0.850 0.380 !       1.93 eA-3
C108 0.079 0.352 0.034 !       1.86 eA-3
C109 0.828 0.557 0.767 !       1.79 eA-3
C110 0.969 0.595 0.889 !       1.75 eA-3
C111 0.518 0.204 0.592 !       1.74 eA-3
C112 0.907 0.571 0.718 !       1.69 eA-3
C113 0.543 0.241 0.542 !       1.69 eA-3
C114 0.531 0.221 0.639 !       1.69 eA-3
C115 0.440 0.855 0.418 !       1.69 eA-3
C116 0.619 0.098 0.673 !       1.60 eA-3
C117 0.926 0.720 0.891 !       1.57 eA-3
C118 0.563 0.155 0.671 !       1.52 eA-3
C119 0.515 0.098 0.549 !       1.51 eA-3
Q120 0.835 0.461 0.836 !       1.49 eA-3
C121 0.187 0.374 0.237 !       1.45 eA-3
C122 0.797 0.531 0.749 !       1.42 eA-3
C123 0.373 0.846 0.415 !       1.42 eA-3
C124 0.802 0.535 0.801 !       1.41 eA-3
C125 0.357 0.973 0.228 !       1.41 eA-3
C126 0.892 0.534 0.688 !       1.41 eA-3
C127 0.343 0.816 0.443 !       1.40 eA-3
C128 0.248 0.935 0.263 !       1.40 eA-3
C129 0.332 0.927 0.202 !       1.37 eA-3
C130 0.943 0.421 0.058 !       1.36 eA-3
C131 0.624 0.024 0.669 !       1.36 eA-3
Q132 0.111 0.330 0.814 !       1.32 eA-3
C133 0.017 0.385 0.161 !       1.31 eA-3
C134 0.658 0.010 0.712 !       1.30 eA-3
C135 0.451 0.958 0.454 !       1.29 eA-3
C136 0.972 0.535 0.895 !       1.28 eA-3
Q137 0.344 0.141 0.232 !       1.27 eA-3
C138 0.969 0.606 0.769 !       1.26 eA-3
Q139 0.973 0.249 0.062 !       1.26 eA-3
C140 0.841 0.523 0.774 !       1.25 eA-3
C141 0.751 0.638 0.751 !       1.25 eA-3
C142 0.702 0.975 0.729 !       1.25 eA-3
Q143 0.485 0.919 0.595 !       1.25 eA-3
Q144 0.514 0.952 0.373 !       1.25 eA-3
C145 0.158 0.277 0.170 !       1.24 eA-3
C146 0.532 0.196 0.702 !       1.23 eA-3
C147 0.142 0.381 0.013 !       1.23 eA-3
Q148 0.469 0.715 0.228 !       1.22 eA-3
C149 0.844 0.656 0.808 !       1.21 eA-3
C150 0.098 0.262 0.066 !       1.21 eA-3
C151 0.609 0.082 0.516 !       1.21 eA-3
C152 0.063 0.393 0.187 !       1.21 eA-3
Q153 0.485 0.923 0.292 !       1.20 eA-3
C154 0.405 0.191 0.497 !       1.20 eA-3
Q155 0.563 0.807 0.409 !       1.20 eA-3
C156 0.077 0.453 0.205 !       1.20 eA-3
C157 0.376 0.878 0.439 !       1.19 eA-3
Q158 0.202 0.574 0.210 !       1.18 eA-3
C159 0.705 0.536 0.784 !       1.17 eA-3
C160 0.657 0.055 0.641 !       1.16 eA-3
C161 0.909 0.651 0.777 !       1.16 eA-3
C162 0.596 0.865 0.522 !       1.15 eA-3
Q163 0.216 0.219 0.167 !       1.15 eA-3
C164 0.017 0.364 0.182 !       1.14 eA-3
C165 0.593 0.084 0.597 !       1.13 eA-3
Q166 0.404 0.579 0.391 !       1.13 eA-3
C167 0.314 0.894 0.361 !       1.12 eA-3
Q168 0.174 0.575 0.292 !       1.12 eA-3
C169 0.128 0.284 0.097 !       1.12 eA-3
Q170 0.220 0.373 0.776 !       1.11 eA-3
Q171 0.798 0.263 0.110 !       1.11 eA-3
Q172 1.001 0.492 0.154 !       1.11 eA-3
C173 0.890 0.515 0.751 !       1.11 eA-3
Q174 0.238 0.331 0.202 !       1.10 eA-3
C175 0.345 0.712 0.376 !       1.10 eA-3
C176 0.655 0.288 0.624 !       1.10 eA-3
Q177 0.562 0.015 0.090 !       1.10 eA-3
C178 0.469 0.053 0.513 !       1.10 eA-3
Q179 0.612 0.331 0.404 !       1.09 eA-3
Q180 0.700 0.716 0.339 !       1.09 eA-3
Q181 0.029 0.600 0.364 !       1.09 eA-3
Q182 0.141 0.827 0.796 !       1.09 eA-3
C183 0.109 0.236 0.137 !       1.09 eA-3
Q184 0.374 0.161 0.433 !       1.09 eA-3
C185 0.930 0.512 0.714 !       1.08 eA-3
C186 0.031 0.541 0.982 !       1.08 eA-3
Q187 0.204 0.926 0.297 !       1.07 eA-3
Q188 0.535 0.037 0.802 !       1.07 eA-3
Q189 0.310 0.807 0.637 !       1.07 eA-3
Q190 0.827 0.641 0.376 !       1.07 eA-3
C191 0.406 0.744 0.315 !       1.06 eA-3
Q192 0.735 0.339 0.660 !       1.06 eA-3
Q193 0.706 0.593 0.857 !       1.05 eA-3
Q194 0.672 0.639 0.629 !       1.05 eA-3
Q195 0.048 0.155 0.554 !       1.05 eA-3
Q196 0.655 0.908 0.565 !       1.04 eA-3
Q197 0.687 0.924 0.595 !       1.04 eA-3
C198 0.578 0.015 0.471 !       1.04 eA-3
C199 0.656 0.070 0.592 !       1.04 eA-3
;
_refine_diff_density_max         0.478
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         7503
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1422
_refine_ls_R_factor_gt           0.0685
_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^)+(0.0806P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1391
_refine_ls_wR_factor_ref         0.1636
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4149
_reflns_number_total             7503
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01178a2.cif
_cod_data_source_block           huj4_0m_sq
_cod_database_code               7241282
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.963
_shelx_estimated_absorpt_t_min   0.810
_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, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C15) \\sim Ueq, Uanis(C14) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
3. Rigid body (RIGU) restrains
 C13, N1, C15, C14
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4.a Riding coordinates:
 O9(H9A,H9B)
4.b Free rotating group:
 O14(H14D,H14E)
4.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C13(H13), C16(H16), C19(H19), C20(H20), C23(H23), C24(H24),
 C25(H25), C28(H28), C29(H29)
4.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C)
4.e Idealised tetrahedral OH refined as rotating group:
 O11(H11)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'