Synthesis, structures, magnetic and electric properties of four new coordination polymers constructed with heterocyclic nitrogen ligands and multidentate organic acid
Yang, Ru-Xia; Lan, Hai-Ming; Zhu, Peng-Yin; Yang, Li-Zhen; Yu, Yu-Ming; Wang, Lu-Lu; Wang, Duo-Zhi; Inorganica Chimica Acta 506 (2020) 119410–; doi:10.1016/j.ica.2019.119410

data_1564966
_publ_section_title
;
 Synthesis, structures, magnetic and electric properties of four new
 coordination polymers constructed with heterocyclic nitrogen ligands and
 multidentate organic acid
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119410
_journal_paper_doi               10.1016/j.ica.2019.119410
_journal_volume                  506
_journal_year                    2020
_chemical_formula_moiety         'C44 H33 Mn N13 O6, 2(H2 O)'
_chemical_formula_sum            'C44 H37 Mn N13 O8'
_chemical_formula_weight         930.80
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                86.0840(10)
_cell_angle_beta                 75.619(2)
_cell_angle_gamma                89.8750(10)
_cell_formula_units_Z            2
_cell_length_a                   9.8545(2)
_cell_length_b                   11.21700(10)
_cell_length_c                   19.5315(4)
_cell_measurement_reflns_used    28215
_cell_measurement_temperature    119.99(10)
_cell_measurement_theta_max      74.1150
_cell_measurement_theta_min      4.4390
_cell_volume                     2086.19(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_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_environment      N~2~
_diffrn_ambient_temperature      119.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -32.00  89.00   0.50    0.50    --    0.00  38.00 -90.00  242
  2  \w    -89.00  32.00   0.50    0.50    --    0.00 -38.00 -90.00  242
  3  \w    -37.00  89.00   0.50    0.50    --    0.00  82.00  30.00  252
  4  \w      6.00 126.00   0.50    1.20    --   95.80 -45.00  30.00  240
  5  \w      6.00 126.00   0.50    1.20    --   95.80 -61.00-120.00  240
  6  \w      6.00 133.00   0.50    1.20    --   95.80 -82.00   0.00  254
  7  \w      6.00 133.00   0.50    1.20    --   95.80 -82.00  30.00  254
  8  \w      6.00 133.00   0.50    1.20    --   95.80 -82.00 -90.00  254
  9  \w      6.00 133.00   0.50    1.20    --   95.80 -82.00-120.00  254
 10  \w     64.00 185.00   0.50    1.20    --   95.80  40.00-100.09  242
 11  \w     64.00 185.00   0.50    1.20    --   95.80  42.00  68.83  242
 12  \w      6.00 126.00   0.50    1.20    --   95.80 -61.00  30.00  240
 13  \w      6.00 133.00   0.50    1.20    --   95.80 -82.00 -60.00  254
 14  \w      6.00 133.00   0.50    1.20    --   95.80 -82.00  90.00  254
 15  \w      6.00 133.00   0.50    1.20    --   95.80 -82.00-180.00  254
 16  \w     58.00 185.00   0.50    1.20    --   95.80  82.00   0.00  254
 17  \w     65.00 185.00   0.50    1.20    --   95.80  43.00 -36.21  240
 18  \w     59.00 185.00   0.50    1.20    --   95.80  30.00-180.00  252
 19  \w    -89.00  37.00   0.50    0.50    --    0.00 -82.00  60.00  252
 20  \w    -32.00  81.00   0.50    0.50    --    0.00  38.00-150.00  226
 21  \w    -30.00  89.00   0.50    0.50    --    0.00  57.00 120.00  238
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1579749000
_diffrn_orient_matrix_UB_12      -0.0139285000
_diffrn_orient_matrix_UB_13      -0.0325116000
_diffrn_orient_matrix_UB_21      0.0261918000
_diffrn_orient_matrix_UB_22      -0.0080578000
_diffrn_orient_matrix_UB_23      0.0747274000
_diffrn_orient_matrix_UB_31      -0.0201248000
_diffrn_orient_matrix_UB_32      -0.1367412000
_diffrn_orient_matrix_UB_33      0.0046834000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            40322
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.465
_diffrn_reflns_theta_min         3.951
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    3.189
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75455
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_description       block
_exptl_crystal_F_000             962
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.977
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         8285
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0514P)^2^+2.1345P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1127
_refine_ls_wR_factor_ref         0.1141
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7893
_reflns_number_total             8285
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            4.cif
_cod_data_source_block           2-yrx-1
_cod_database_code               1564966
_shelx_estimated_absorpt_t_max   0.721
_shelx_estimated_absorpt_t_min   0.469
_reflns_odcompleteness_completeness 99.46
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O8) = Uanis(O8A)
3. Others
 Fixed Sof: N13(0.67) H13A(0.67) H13B(0.67) N13A(0.33) H13C(0.33) H13D(0.33)
 H21(0.67) H24(0.33) O8(0.8) H8A(0.8) H8B(0.8) O8A(0.2) H8AA(0.2) H8AB(0.2)
4.a Free rotating group:
 O7(H7A,H7B), O8(H8A,H8B), O8A(H8AA,H8AB)
4.b Rotating group:
 O1(H1A,H1B), O6(H6A,H6B), N13(H13A,H13B)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C12(H12), C14(H14),
 C15(H15), C16(H16), C17(H17), C21(H21), C22(H22), C24(H24), C25(H25), C27(H27),
  C29(H29), C30(H30), C31(H31), C32(H32), C35(H35), C36(H36), C38(H38),
 C40(H40), C41(H41), C42(H42), C43(H43)
4.d X=CH2 refined with riding coordinates:
 N13A(H13C,H13D)
;
_shelx_res_checksum              61970
_shelx_hkl_checksum              64550
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.820
_oxdiff_exptl_absorpt_empirical_full_min 0.485