The synthesis, structure, topology and catalytic application of a novel cubane-based copper(ii) metal-organic framework derived from a flexible amido tripodal acid.
Karmakar, Anirban; Oliver, Clive L.; Roy, Somnath; Öhrström, Lars; Dalton transactions (Cambridge, England : 2003) 44 (2015) 10156–10165; doi:10.1039/c4dt03087g

data_7033811
_publ_section_title
;
 The synthesis, structure, topology and catalytic application of a novel
 cubane-based copper(ii) metal-organic framework derived from a flexible
 amido tripodal acid.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10156
_journal_page_last               10165
_journal_paper_doi               10.1039/c4dt03087g
_journal_volume                  44
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C20 H29 Cu2 N3 O13'
_chemical_formula_sum            'C20 H29 Cu2 N3 O13'
_chemical_formula_weight         646.54
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-12-18
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2014-12-24 deposited with the CCDC.
2015-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.9809(12)
_cell_length_b                   18.9809(12)
_cell_length_c                   17.5707(12)
_cell_measurement_temperature    100(2)
_cell_volume                     6330.3(7)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_av_unetI/netI     0.0632
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            40233
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.682
_diffrn_reflns_theta_min         1.517
_exptl_absorpt_coefficient_mu    1.401
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6758
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/2 (Bruker,2014) was used for absorption correction. wR2(int) was 0.0812 before and 0.0576 after correction. The Ratio of minimum to maximum transmission is 0.9058. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_description       block
_exptl_crystal_F_000             2656
_exptl_crystal_size_max          0.264
_exptl_crystal_size_mid          0.228
_exptl_crystal_size_min          0.193
_refine_diff_density_max         2.070
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.130
_refine_ls_abs_structure_details
;
 Flack x determined using 2832 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.034(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         9790
_refine_ls_number_restraints     184
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0566
_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^)+(0.1093P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1588
_refine_ls_wR_factor_ref         0.1712
_reflns_Friedel_coverage         0.783
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                7629
_reflns_number_total             9790
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03087g2.cif
_cod_data_source_block           fp432212_sq
_cod_depositor_comments          'Adding full bibliography for 7033811.cif.'
_cod_original_cell_volume        6330.3(9)
_cod_database_code               7033811
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.774
_shelx_estimated_absorpt_t_min   0.709
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 N1-H1
 0.87 with sigma of 0.02
 H2-N2
 0.87 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N3 \\sim C16 \\sim C17 \\sim C18 \\sim O8 \\sim O9 \\sim N3A \\sim C16A \\sim
C17A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
O9 \\sim C18 \\sim O8 \\sim O9A \\sim C18A \\sim O8A: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 N3, C16, C17, C18, O8, O9, N3A, C16A, C17A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O9, C18, O8, O9A, C18A, O8A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{N3, C16, C17, C18, O8, O9}
as
{N3A, C16A, C17A, C18A, O8A, O9A}
6. Others
 Sof(N3A)=Sof(H3A)=Sof(C16A)=Sof(H16A)=Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=
 Sof(C18A)=Sof(O8A)=Sof(H8AA)=Sof(O9A)=1-FVAR(1)
 Sof(N3)=Sof(H3)=Sof(C16)=Sof(H16)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=
 Sof(C18)=Sof(O8)=Sof(H8A)=Sof(O9)=FVAR(1)
7.a Rotating group:
 OW1(HW1A,HW1B), OW2(HW2A,HW2B)
7.b Ternary CH refined with riding coordinates:
 C8(H8), C12(H12), C16(H16), C16A(H16A)
7.c Aromatic/amide H refined with riding coordinates:
 C2(H2A), C4(H4), C6(H6), N3(H3), N3A(H3A)
7.d Tetrahedral OH refined with riding coordinates:
 O8(H8A), O8A(H8AA)
7.e Idealised Me refined as rotating group:
 C0AA(H0AA,H0AB,H0AC), C1M1(H1MA,H1MB,H1MC), C1M2(H1MD,H1ME,H1MF), C13(H13A,
 H13B,H13C), C17(H17A,H17B,H17C), C17A(H17D,H17E,H17F)
;
_shelx_res_checksum              11535
_shelx_fab_checksum              54925
_olex2_submission_special_instructions 'No special instructions were received'