Two Types of Cu-Ln Heterometallic Coordination Polymers with 2-Hydroxyisophthalate: Syntheses, Structures, and Magnetic Properties
Wang, Kai; Chen, Zi-Lu; Zou, Hua-Hong; Zhang, Zhong; Sun, Wei-Yin; Liang, Fu-Pei; Crystal Growth & Design 15 (2015) 2883–; doi:10.1021/acs.cgd.5b00327

data_4513004
_publ_section_title
;
 Two Types of Cu-Ln Heterometallic Coordination Polymers with
 2-Hydroxyisophthalate: Syntheses, Structures, and Magnetic Properties
;
_journal_issue                   6
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              2883
_journal_paper_doi               10.1021/acs.cgd.5b00327
_journal_volume                  15
_journal_year                    2015
_chemical_formula_moiety         'C24 H19 Cu3 O20 Tb, H2 O'
_chemical_formula_sum            'C24 H21 Cu3 O21 Tb'
_chemical_formula_weight         994.95
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-04-04
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                116.174(2)
_cell_angle_beta                 96.5555(18)
_cell_angle_gamma                92.0057(18)
_cell_formula_units_Z            2
_cell_length_a                   9.87924(19)
_cell_length_b                   12.1357(3)
_cell_length_c                   12.7211(3)
_cell_measurement_reflns_used    12631
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      28.4550
_cell_measurement_theta_min      2.9411
_cell_volume                     1353.57(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean 15.9784
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -14.00   19.00   0.7500   20.2800
omega____ theta____ kappa____ phi______ frames
    -      -20.2889  -99.0000   30.0000 44

  2 omega  -20.00    5.50   0.7500   20.2800
omega____ theta____ kappa____ phi______ frames
    -      -20.2889  -99.0000   90.0000 34

  3 omega    5.00   90.50   0.7500   20.2800
omega____ theta____ kappa____ phi______ frames
    -       21.3827   57.0000  -60.0000 114

  4 omega    2.00   89.00   0.7500   20.2800
omega____ theta____ kappa____ phi______ frames
    -       21.3827   57.0000   30.0000 116

  5 omega   41.00   87.50   0.7500   20.2800
omega____ theta____ kappa____ phi______ frames
    -       21.3827   57.0000   90.0000 62

  6 omega   47.00   76.25   0.7500   20.2800
omega____ theta____ kappa____ phi______ frames
    -       21.3827   57.0000 -120.0000 39

  7 omega  -45.00   53.25   0.7500   20.2800
omega____ theta____ kappa____ phi______ frames
    -       21.3827  -80.0000  171.0000 131

  8 omega  -91.00    2.00   0.7500   20.2800
omega____ theta____ kappa____ phi______ frames
    -      -20.2889  -57.0000    0.0000 124

  9 omega -100.00  -36.25   0.7500   20.2800
omega____ theta____ kappa____ phi______ frames
    -      -20.2889 -178.0000  -30.0000 85

 10 omega -102.00  -35.25   0.7500   20.2800
omega____ theta____ kappa____ phi______ frames
    -      -20.2889  178.0000  120.0000 89

 11 omega  -45.00   12.00   0.7500   20.2800
omega____ theta____ kappa____ phi______ frames
    -      -20.2889  -80.0000  171.0000 76

 12 omega   -2.00   91.00   0.7500   20.2800
omega____ theta____ kappa____ phi______ frames
    -       21.3827   57.0000 -150.0000 124

 13 omega  -49.00   44.00   0.7500   20.2800
omega____ theta____ kappa____ phi______ frames
    -       21.3827  -57.0000  -60.0000 124

 14 omega  -44.00   49.00   0.7500   20.2800
omega____ theta____ kappa____ phi______ frames
    -      -20.2889   57.0000  150.0000 124

 15 omega  -51.00   54.00   0.7500   20.2800
omega____ theta____ kappa____ phi______ frames
    -       21.3827  -77.0000  -90.0000 140

 16 omega  -20.00   64.75   0.7500   20.2800
omega____ theta____ kappa____ phi______ frames
    -       21.3827  -99.0000   60.0000 113
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0005722000
_diffrn_orient_matrix_UB_12      0.0347453000
_diffrn_orient_matrix_UB_13      -0.0325125000
_diffrn_orient_matrix_UB_21      -0.0538164000
_diffrn_orient_matrix_UB_22      -0.0414326000
_diffrn_orient_matrix_UB_23      -0.0424208000
_diffrn_orient_matrix_UB_31      -0.0487305000
_diffrn_orient_matrix_UB_32      0.0368329000
_diffrn_orient_matrix_UB_33      0.0329491000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            25089
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.95
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.011
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93840
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
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    2.441
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             970
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.793
_refine_diff_density_min         -3.146
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         4757
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0433
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0660P)^2^+13.1770P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1251
_refine_ls_wR_factor_ref         0.1276
_reflns_number_gt                4374
_reflns_number_total             4757
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg5b00327_si_005.cif
_cod_data_source_block           0723-lfp-wk-13071503f
_cod_depositor_comments
'Adding full bibliography for 4513003--4513006.cif.'
_cod_original_cell_volume        1353.57(5)
_cod_database_code               4513004
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 O20-H20a = O20-H20b
 0.85 with sigma of 0.01
 H20a-H20b
 1.4 with sigma of 0.02
 O18-H18b = O18-H18a
 0.85 with sigma of 0.01
 H18b-H18a
 1.4 with sigma of 0.02
 O19-H19a = O19-H19b
 0.85 with sigma of 0.01
 H19a-H19b
 1.4 with sigma of 0.02
 O21-H21a = O21-H21b
 0.85 with sigma of 0.01
 H21a-H21b
 1.4 with sigma of 0.02
 O16-H16a
 0.85 with sigma of 0.01
 H20a-H20b
 1.4 with sigma of 0.02
 O17-H17b = O17-H17a
 0.85 with sigma of 0.01
 H17b-H17a
 1.4 with sigma of 0.02
 O16-H16a = O16-H16b
 0.85 with sigma of 0.01
 H16a-H16b
 1.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C11(H11), C12(H12), C13(H13), C19(H19), C20(H20),
 C21(H21)
;
_olex2_submission_special_instructions 'No special instructions were received'