A novel highly efficient adsorbent {[Co4(L)2(μ3-OH)2(H2O)3(4,4′-bipy)2]·(H2O)2}n: Synthesis, crystal structure, magnetic and arsenic (V) absorption capacity
Zhang, Chong; Xiao, Yu; Qin, Yan; Sun, Quanchun; Zhang, Shuhua; Journal of Solid State Chemistry 261 (2018) 22–30; doi:10.1016/j.jssc.2018.02.012

data_1561138
_publ_section_title
;
 A novel highly efficient adsorbent
 {[Co4(L)2(\m3-OH)2(H2O)3(4,4&#x2032;-bipy)2]&#x00B7;(H2O)2}n: Synthesis,
 crystal structure, magnetic and arsenic (V) absorption capacity
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              22
_journal_page_last               30
_journal_paper_doi               10.1016/j.jssc.2018.02.012
_journal_volume                  261
_journal_year                    2018
_chemical_formula_moiety         'C64 H56 Co4 N6 O19 S2, 2(H2 O)'
_chemical_formula_sum            'C64 H60 Co4 N6 O21 S2'
_chemical_formula_weight         1549.02
_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     direct
_cell_angle_alpha                62.636(5)
_cell_angle_beta                 80.488(4)
_cell_angle_gamma                80.348(4)
_cell_formula_units_Z            2
_cell_length_a                   14.0139(7)
_cell_length_b                   16.7666(6)
_cell_length_c                   16.8339(9)
_cell_measurement_reflns_used    11206
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.0470
_cell_measurement_theta_min      3.5090
_cell_volume                     3445.5(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, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0233
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -20.00   61.00   1.0000   26.5000
omega____ theta____ kappa____ phi______ frames
    -       18.6266  -99.0000   30.0000 81

  2 omega  -44.00    9.00   1.0000   26.5000
omega____ theta____ kappa____ phi______ frames
    -      -18.7048  -77.0000   60.0000 53

  3 omega  -88.00    3.00   1.0000   26.5000
omega____ theta____ kappa____ phi______ frames
    -      -18.7048  -57.0000  -90.0000 91

  4 omega  -88.00    3.00   1.0000   26.5000
omega____ theta____ kappa____ phi______ frames
    -      -18.7048  -57.0000  150.0000 91

  5 omega  -40.00   45.00   1.0000   26.5000
omega____ theta____ kappa____ phi______ frames
    -      -18.7048   57.0000 -180.0000 85

  6 omega  -86.00   -2.00   1.0000   26.5000
omega____ theta____ kappa____ phi______ frames
    -      -18.7048  -38.0000    0.0000 84

  7 omega  -49.00   50.00   1.0000   26.5000
omega____ theta____ kappa____ phi______ frames
    -      -18.7048   77.0000   60.0000 99

  8 omega  -22.00   50.00   1.0000   26.5000
omega____ theta____ kappa____ phi______ frames
    -      -18.7048   57.0000  -60.0000 72

  9 omega  -90.00  -13.00   1.0000   26.5000
omega____ theta____ kappa____ phi______ frames
    -      -18.7048  147.0000  153.4972 77
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0307767000
_diffrn_orient_matrix_UB_12      0.0083361000
_diffrn_orient_matrix_UB_13      -0.0403453000
_diffrn_orient_matrix_UB_21      0.0197898000
_diffrn_orient_matrix_UB_22      -0.0459116000
_diffrn_orient_matrix_UB_23      0.0188030000
_diffrn_orient_matrix_UB_31      -0.0363809000
_diffrn_orient_matrix_UB_32      -0.0108175000
_diffrn_orient_matrix_UB_33      -0.0170991000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0533
_diffrn_reflns_av_unetI/netI     0.0675
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            48573
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         3.388
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.084
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69160
_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_density_diffrn    1.493
_exptl_crystal_description
;
;
_exptl_crystal_F_000             1588
_refine_diff_density_max         0.766
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     928
_refine_ls_number_reflns         14033
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0503
_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^)+(0.0452P)^2^+1.6926P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1133
_refine_ls_wR_factor_ref         0.1337
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9883
_reflns_number_total             14033
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            JSSC-2018-261-22.cif
_cod_data_source_block           co
_cod_original_cell_volume        3445.4(3)
_cod_database_code               1561138
_chemical_oxdiff_formula         'C1 H1 O1 N1 Co1'
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H21A,H21B} of O21, {H20A,H20B} of O20, {H6A,H6B} of O6,
  All C(H,H) groups
 At 1.5 times of:
  {H8C,H8D} of O8
2. Restrained distances
 O5-H5
 0.86 with sigma of 0.01
 O9-H9
 0.86 with sigma of 0.01
3. Others
 Sof(S2')=Sof(O12')=Sof(O13')=Sof(O14')=1-FVAR(1)
 Sof(S2)=Sof(O12)=Sof(O13)=Sof(O14)=FVAR(1)
4.a Riding coordinates:
 O6(H6A,H6B), O21(H21A,H21B), O20(H20A,H20B)
4.b Rotating group:
 O8(H8C,H8D)
4.c Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C37(H37A,H37B), C8(H8A,H8B), C30(H30A,H30B)
4.d Aromatic/amide H refined with riding coordinates:
 C51(H51), C52(H52), C47(H47), C48(H48), C3(H3), C55(H55), C54(H54), C56(H56),
 C6(H6), C14(H14), C39(H39), C41(H41), C4(H4), C61(H61), C53(H53), C63(H63),
 C40(H40), C45(H45), C31(H31), C46(H46), C42(H42), C32(H32), C34(H34), C26(H26),
  C57(H57), C20(H20), C58(H58), C35(H35), C25(H25), C17(H17), C19(H19), C5(H5A),
  C28(H28), C11(H11), C27(H27), C18(H18), C13(H13), C10(H10), C62(H62), C64(H64)
;