Complex three-dimensional lanthanide metal‒organic frameworks with variable coordination spheres based on pyrazine-2,3,5,6-tetracarboxylate
Ingram, Conrad W.; Kibakaya, Geoffrey; Bacsa, John; Mathis,II, Stephan R.; Holder, Alvin A.; Rambaran, Varma H.; Dennis, Brandon; Castaneda, Esmeralda; Robbins, Julianne S.; John Zhang, Z.; CrystEngComm 17 (2015) 5377–; doi:10.1039/C4CE02564D

data_7220525
_publ_section_title
;
 Complex three-dimensional lanthanide metal--organic frameworks with
 variable coordination spheres based on pyrazine-2,3,5,6-tetracarboxylate
;
_journal_issue                   29
_journal_name_full               CrystEngComm
_journal_page_first              5377
_journal_paper_doi               10.1039/C4CE02564D
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C24 H22 N6 O35 Tb4, 10(H2 O)'
_chemical_formula_sum            'C24 H42 N6 O45 Tb4'
_chemical_formula_weight         1770.31
_chemical_name_systematic
;
 ?
;
_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   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2014-11-04
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.11.03 svn.r3071 for OlexSys, GUI svn.r4932)
;
_audit_update_record
;
2015-04-30 deposited with the CCDC.
2015-05-19 downloaded from the CCDC.
;
_cell_angle_alpha                88.568(3)
_cell_angle_beta                 86.325(4)
_cell_angle_gamma                81.382(3)
_cell_formula_units_Z            2
_cell_length_a                   8.5627(15)
_cell_length_b                   14.078(3)
_cell_length_c                   20.297(4)
_cell_measurement_reflns_used    2805
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      30.395
_cell_measurement_theta_min      2.410
_cell_volume                     2413.8(8)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       'APEX2 v2013.2-4 (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.32B (Bruker, 2013)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1810
_diffrn_reflns_av_unetI/netI     1.0164
_diffrn_reflns_laue_measured_fraction_full 0.991
_diffrn_reflns_laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            19021
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.732
_diffrn_reflns_theta_min         1.463
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           30
_diffrn_source_voltage           45
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.923
_exptl_absorpt_correction_T_max  0.746039
_exptl_absorpt_correction_T_min  0.458887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0676 before and 0.0360 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.0819 before and 0.0395 after correction.
 The Ratio of minimum to maximum transmission is 0.62.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 19279 reflections, Rint = 0.0404
 (4727 with I > 3sig(I), Rint = 0.0329)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.436
_exptl_crystal_description       needle
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.833
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.032
_refine_diff_density_max         4.694
_refine_diff_density_min         -4.535
_refine_diff_density_rms         0.606
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     787
_refine_ls_number_reflns         10146
_refine_ls_number_restraints     874
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.2457
_refine_ls_R_factor_gt           0.1347
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1177P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2557
_refine_ls_wR_factor_ref         0.2983
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3676
_reflns_number_total             10146
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ce02564d2.cif
_cod_data_source_block           b420
_cod_depositor_comments
'Adding full bibliography for 7220524--7220525.cif.'
_cod_original_cell_volume        2413.9(7)
_cod_database_code               7220525
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.833
_shelx_estimated_absorpt_t_min   0.083
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 O6_$2-H2WB
 1.7 with sigma of 0.01
 O16W-H1WB
 1.7 with sigma of 0.02
 O6_$5-H5WB
 1.9 with sigma of 0.02
 O18W-H6WB
 1.685 with sigma of 0.02
 O11_$6-H6WA
 1.8 with sigma of 0.02
 O23_$8-H7WB
 1.9 with sigma of 0.02
 O10W_$1-H3WA
 1.7 with sigma of 0.02
 H5WA-O10_$5
 1.9 with sigma of 0.02
 H5WB-O6_$5
 1.9 with sigma of 0.02
 H5WB-O5W
 0.995 with sigma of 0.005
 O6_$5-H5WB
 2.1 with sigma of 0.02
 O21W-H21B = O21W-H21A
 0.985 with sigma of 0.005
 H21B-H21A
 1.555 with sigma of 0.005
 O20_$9-H9WB
 1.923 with sigma of 0.003
 O18_$8-H9WA
 1.85 with sigma of 0.02
 H1WA-O12W_$4
 1.7 with sigma of 0.02
 O14_$6-H10A = O12W_$4-H10B
 1.8 with sigma of 0.02
 O12W_$4-H10B = O14_$6-H10A
 1.9 with sigma of 0.02
 O9W-H9WB = O9W-H9WA = O10W-H10A = O10W-H10B
 0.985 with sigma of 0.005
 H9WB-H9WA = H10A-H10B
 1.548 with sigma of 0.01
 O5W-H5WB = O5W-H5WA = O6W-H6WB = O6W-H6WA = O7W-H7WA = O7W-H7WB = O8W-H8WA =
 O8W-H8WB
 0.975 with sigma of 0.005
 O12-H8WB = H8WA-O7_$6
 1.9 with sigma of 0.02
 O22_$3-H4WB = O19W_$4-H4WA
 1.7 with sigma of 0.02
 O4W_$7-H7WA
 1.9 with sigma of 0.02
 O1W-H1WA = O1W-H1WB = O2W-H2WA = O3W-H3WB = O3W-H3WA = O4W-H4WB = O4W-H4WA
 0.975 with sigma of 0.004
 H1WB-H1WA = H2WA-H2WB = H3WB-H3WA = H4WB-H4WA = H5WB-H5WA = H6WB-H6WA = H7WB-
 H7WA = H8WA-H8WB
 1.548 with sigma of 0.007
3. Uiso/Uaniso restraints and constraints
Uanis(C12) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(N3) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(C11) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O8) \\sim
Ueq, Uanis(C7) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(N6)
\\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O12) \\sim Ueq,
Uanis(C8) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(O5)
\\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O10) \\sim Ueq: with
sigma of 0.002 and sigma for terminal atoms of 0.002
Uanis(C15) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(O13)
\\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C16) \\sim Ueq,
Uanis(O15) \\sim Ueq, Uanis(O16) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
Uanis(O21) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(O17)
\\sim Ueq, Uanis(O18) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(N4) \\sim Ueq,
Uanis(C24) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(O20)
\\sim Ueq, Uanis(O19) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C22) \\sim Ueq,
Uanis(C23) \\sim Ueq, Uanis(O23) \\sim Ueq, Uanis(O24) \\sim Ueq, Uanis(O22)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O2) \\sim
Ueq, Uanis(C3) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(O3)
\\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.005
Uanis(O1W) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
Uanis(O1W) \\sim Ueq, Uanis(O8W) \\sim Ueq, Uanis(O21W) \\sim Ueq, Uanis(O2W)
\\sim Ueq, Uanis(O3W) \\sim Ueq, Uanis(O19W) \\sim Ueq, Uanis(O7W) \\sim Ueq,
Uanis(O18W) \\sim Ueq, Uanis(O11W) \\sim Ueq, Uanis(O12W) \\sim Ueq, Uanis(O9W)
\\sim Ueq, Uanis(O4W) \\sim Ueq, Uanis(O17W) \\sim Ueq, Uanis(O15W) \\sim Ueq,
Uanis(O20W) \\sim Ueq, Uanis(O10W) \\sim Ueq, Uanis(O13W) \\sim Ueq,
Uanis(O14W) \\sim Ueq, Uanis(O16W) \\sim Ueq, Uanis(O5W) \\sim Ueq, Uanis(O6W)
\\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(C20) = Uanis(C23)
4. Rigid body (RIGU) restrains
 O3, C4, O4, C3
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O6, O5, C10, C9
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C9, N5, C8, C12, N6, C7, C6
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C8, C12, O9, O10
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O9, C12, O10, C8
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C7, C11, O12
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 N2, C13, C14, O13, O14, C15, C16, O15, O16
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O2, C1, C2, O1, C3, N1, C4, O3, O4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N2, C13, C14, O13, O14, C15, C16, O15, O16
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C7, C5, C6, O7, O8, N5, C11, N6, C9, O11, O12, C8, C10, C12, O5, O6, O9, O10
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O21, C23, C20, N3, C19, C18, N4, C21
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O19, C17, C18, O17, O18, C19, N4, C24, N3, C21, O20, C20, C22, C23, O23, O24,
 O22, O21
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O1W, Tb2
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 Tb2, O4W
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5.a Free rotating group:
 O15W(H15A,H15B), O16W(H16A,H16B), O19W(H19A,H19B), O17W(H17A,H17B), O18W(H18A,
 H18B), O14W(H14W)
5.b Rotating group:
 O20W(H20A,H20B), O21W(H21A,H21B)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a loop with paratone oil'
_olex2_submission_original_sample_id B420
_olex2_submission_special_instructions 'No special instructions were received'