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_7220524
_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 Gd4 N6 O35, 10(H2 O)'
_chemical_formula_sum            'C24 H42 Gd4 N6 O45'
_chemical_formula_weight         1763.63
_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     iterative
_audit_creation_date             2014-11-07
_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                88.5392(17)
_cell_angle_beta                 86.4998(15)
_cell_angle_gamma                81.2519(16)
_cell_formula_units_Z            2
_cell_length_a                   8.5607(10)
_cell_length_b                   14.1023(17)
_cell_length_c                   20.294(2)
_cell_measurement_reflns_used    5744
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      33.233
_cell_measurement_theta_min      2.503
_cell_volume                     2416.7(5)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'APEX2 v2011.2-4 (Bruker, 2011)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans with a narrow frame width'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0571
_diffrn_reflns_av_unetI/netI     0.0648
_diffrn_reflns_laue_measured_fraction_full 0.992
_diffrn_reflns_laue_measured_fraction_max 0.915
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            24173
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.915
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         33.346
_diffrn_reflns_theta_min         2.011
_diffrn_source                   'sealed tube'
_diffrn_source_current           30
_diffrn_source_voltage           45
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.552
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.4305
_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 0.0637 before and 0.0418 after correction.
 The Ratio of minimum to maximum transmission is 0.66.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.0781 before and 0.0591 after correction.
 The Ratio of minimum to maximum transmission is 0.66.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 66002 reflections, Rint = 0.0431
 (34334 with I > 3sig(I), Rint = 0.0392)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.424
_exptl_crystal_description       needle
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.394
_exptl_crystal_size_mid          0.146
_exptl_crystal_size_min          0.108
_refine_diff_density_max         4.712
_refine_diff_density_min         -5.877
_refine_diff_density_rms         0.384
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     814
_refine_ls_number_reflns         17134
_refine_ls_number_restraints     238
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0570
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0853P)^2^+17.1055P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1455
_refine_ls_wR_factor_ref         0.1516
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14301
_reflns_number_total             17134
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ce02564d2.cif
_cod_data_source_block           twin4
_cod_depositor_comments
'Adding full bibliography for 7220524--7220525.cif.'
_cod_original_cell_volume        2416.6(5)
_cod_database_code               7220524
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All H(H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O1W-H1WA = O1W-H1WB = O2W-H2WA = O3W-H3WB = O3W-H3WA = O4W-H4WB = O4W-H4WA
 0.985 with sigma of 0.01
 O5W-H5WB = O5W-H5WA = O6W-H6WB = O6W-H6WA = O7W-H7WA = O7W-H7WB = O8W-H8WA =
 O8W-H8WB
 0.985 with sigma of 0.01
 H1WB-H1WA = H2WA-H2WB = H3WB-H3WA = H4WB-H4WA = H5WB-H5WA = H6WB-H6WA = H7WB-
 H7WA = H8WA-H8WB
 1.548 with sigma of 0.01
 O9W-H9WB = O9W-H9WA = O10W-H10A = O10W-H10B = O11W-H11B = O11W-H11A = O12W-
 H12B = O12W-H12A
 0.985 with sigma of 0.01
 H9WB-H9WA = H10A-H10B = H11A-H11B = H12B-H12A
 1.548 with sigma of 0.01
 O6_$8-H2WB
 1.7 with sigma of 0.01
 O16W-H1WB
 1.7 with sigma of 0.02
 H1WA-O12W_$10
 1.7 with sigma of 0.02
 O22_$9-H4WB = O19W_$10-H4WA
 1.7 with sigma of 0.02
 O6_$2-H5WB
 1.9 with sigma of 0.02
 O18W-H6WB
 1.685 with sigma of 0.02
 O11_$3-H6WA
 1.8 with sigma of 0.02
 O4W_$4-H7WA
 1.9 with sigma of 0.02
 O23_$5-H7WB
 1.9 with sigma of 0.02
 O12-H8WB = H8WA-O7_$3
 1.9 with sigma of 0.02
 O18_$5-H9WA
 1.85 with sigma of 0.02
 O20_$6-H9WB
 1.923 with sigma of 0.003
 O10W_$1-H3WA
 1.7 with sigma of 0.02
 O14_$3-H10A = O12W_$10-H10B
 1.8 with sigma of 0.02
 O12W_$10-H10B = O14_$3-H10A
 1.9 with sigma of 0.02
 O21_$6-H11B
 1.88 with sigma of 0.02
 O13_$7-H11A
 1.9 with sigma of 0.02
 H12A-O24_$4
 1.9 with sigma of 0.01
 H5WA-O10_$2
 1.9 with sigma of 0.02
 H5WB-O6_$2
 1.9 with sigma of 0.02
 H5WB-O5W
 0.995 with sigma of 0.005
 O6_$2-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
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
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
 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
 C7, C11, O12
 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), O13W(H13A,H13B), O19W(H19A,H19B), O17W(H17A,
 H17B), O18W(H18A,H18B), O14W(H14A,H14B)
5.b Rotating group:
 O20W(H20A,H20B)
;
_shelx_res_checksum              10857
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a loop with paratone oil'
_olex2_submission_special_instructions 'No special instructions were received'