A rare 3D chloro-laced Mn(II) metal-organic framework to show sensitive probing effect to Hg 2+
Ming, Mei; Bai, Na; Journal of Solid State Chemistry 254 (2017) 9–13; doi:10.1016/j.jssc.2017.07.003

data_1560360
_publ_contact_author_name
;
;
_publ_section_title
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 A rare 3D chloro-laced Mn(II) metal-organic framework to show sensitive
 probing effect to Hg 2+
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              9
_journal_page_last               13
_journal_paper_doi               10.1016/j.jssc.2017.07.003
_journal_volume                  254
_journal_year                    2017
_chemical_formula_moiety         '0.25(C80 H84 Mn4 N12 O20)'
_chemical_formula_sum            'C20 H21 Mn N3 O5'
_chemical_formula_weight         438.34
_space_group_crystal_system      orthorhombic
_space_group_IT_number           54
_space_group_name_Hall           '-P 2a 2ac'
_space_group_name_H-M_alt        'P c c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-06-04
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.267(2)
_cell_length_b                   13.5379(12)
_cell_length_c                   7.4103(7)
_cell_measurement_reflns_used    1374
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      73.2240
_cell_measurement_theta_min      5.4460
_cell_volume                     2033.2(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2740
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega    8.00   41.00   1.0000    4.3800
omega____ theta____ kappa____ phi______ frames
    -       43.1514  -99.0000   90.0000 33

  2 omega   49.00   80.00   1.0000    4.3800
omega____ theta____ kappa____ phi______ frames
    -       43.1514  -99.0000   90.0000 31

  3 omega   33.00   89.00   1.0000   17.5200
omega____ theta____ kappa____ phi______ frames
    -      106.0351  -30.0000  150.0000 56

  4 omega   67.00   95.00   1.0000   17.5200
omega____ theta____ kappa____ phi______ frames
    -      106.0351   15.0000  150.0000 28

  5 omega   88.00  176.00   1.0000   17.5200
omega____ theta____ kappa____ phi______ frames
    -      106.0351   45.0000  120.0000 88

  6 omega   63.00   90.00   1.0000   17.5200
omega____ theta____ kappa____ phi______ frames
    -      106.0351  -30.0000  -90.0000 27

  7 omega   38.00   65.00   1.0000   17.5200
omega____ theta____ kappa____ phi______ frames
    -      106.0351  -45.0000 -150.0000 27

  8 omega    5.00   55.00   1.0000    4.3800
omega____ theta____ kappa____ phi______ frames
    -       43.1514  -99.0000  -30.0000 50

  9 omega  -48.00  -17.00   1.0000    4.3800
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -57.0000 -180.0000 31

 10 omega -107.00  -68.00   1.0000    4.3800
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -57.0000 -180.0000 39
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0735466000
_diffrn_orient_matrix_UB_12      -0.0190826000
_diffrn_orient_matrix_UB_13      0.0405568000
_diffrn_orient_matrix_UB_21      -0.0016174000
_diffrn_orient_matrix_UB_22      0.0915648000
_diffrn_orient_matrix_UB_23      0.1231492000
_diffrn_orient_matrix_UB_31      -0.0192492000
_diffrn_orient_matrix_UB_32      0.0648357000
_diffrn_orient_matrix_UB_33      -0.1623950000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_unetI/netI     0.0496
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            4304
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.068
_diffrn_reflns_theta_max         67.068
_diffrn_reflns_theta_min         4.363
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.597
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.22179
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_description       needle
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.075
_refine_diff_density_min         -0.801
_refine_diff_density_rms         0.143
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         1816
_refine_ls_number_restraints     89
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1150
_refine_ls_R_factor_gt           0.0935
_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^)+(0.1424P)^2^+8.0199P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2353
_refine_ls_wR_factor_ref         0.2548
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1339
_reflns_number_total             1816
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            mmc2.cif
_cod_data_source_block           2
_cod_database_code               1560360
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
2. Restrained distances
 C12-C13
 2.55 with sigma of 0.01
 C10-C11
 1.48 with sigma of 0.01
 N1-C12 = N1-C13
 1.48 with sigma of 0.01
 C10-N1
 1.36 with sigma of 0.01
 O3-C10
 1.2 with sigma of 0.01
 O3-Mn1
 2.26 with sigma of 0.01
 C13-C10 \\sim C10-C12
 with sigma of 0.005
3. Restrained planarity
 O3, N1, C10, C11, C12, C13
 with sigma of 0.005
4. Uiso/Uaniso restraints and constraints
O3 \\sim N1 \\sim C10 \\sim C11 \\sim C12 \\sim C13: within 1.7A with sigma of
0.005 and sigma for terminal atoms of 0.002
C3 \\sim C4 \\sim C5 \\sim C6 \\sim C1 \\sim C2 \\sim N9: within 2A with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(O3) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Others
 Fixed Sof: O3(0.5) N1(0.5) C10(0.5) C11(0.5) H11A(0.5) H11B(0.5) H11C(0.5)
 C12(0.5) H12A(0.5) H12B(0.5) H12C(0.5) C13(0.5) H13A(0.5) H13B(0.5) H13C(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6)
6.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'