Crystal engineering of dichromate pillared hybrid ultramicroporous materials incorporating pyrazole-based ligands
Scott, Hayley S.; Mukherjee, Soumya; Turner, David R.; Polson, Matthew I. J.; Zaworotko, Michael J.; Kruger, Paul E.; CrystEngComm 20 (2018) 1193–; doi:10.1039/C8CE00149A

data_7230121
_publ_section_title
;
 Crystal engineering of dichromate pillared hybrid ultramicroporous
 materials incorporating pyrazole-based ligands
;
_journal_issue                   9
_journal_name_full               CrystEngComm
_journal_page_first              1193
_journal_paper_doi               10.1039/C8CE00149A
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         '0.25(C80 H112 Cr8 Cu4 N32 O28)'
_chemical_formula_sum            'C20 H28 Cr2 Cu N8 O7'
_chemical_formula_weight         660.04
_space_group_crystal_system      tetragonal
_space_group_IT_number           90
_space_group_name_Hall           'P 4ab 2ab'
_space_group_name_H-M_alt        'P 4 21 2'
_symmetry_space_group_name_Hall  'P 4ab 2ab'
_symmetry_space_group_name_H-M   'P 4 21 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-12-20
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2018-01-08 deposited with the CCDC.
2018-02-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.658(2)
_cell_length_b                   18.658(2)
_cell_length_c                   8.6530(17)
_cell_measurement_reflns_used    26973
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      31.951
_cell_measurement_theta_min      1.543
_cell_volume                     3012.3(7)
_computing_cell_refinement       XDS
_computing_data_collection       BluICE
_computing_data_reduction        XDS
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  'Australian Synchrotron'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0840
_diffrn_reflns_av_unetI/netI     0.0463
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            26973
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.951
_diffrn_reflns_theta_min         1.543
_exptl_absorpt_coefficient_mu    1.457
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.4848
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_description       plate
_exptl_crystal_F_000             1348
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.697
_refine_diff_density_min         -0.744
_refine_diff_density_rms         0.153
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.50(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         4800
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.1119
_refine_ls_R_factor_gt           0.0950
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1628P)^2^+3.7012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2611
_refine_ls_wR_factor_ref         0.2747
_reflns_Friedel_coverage         0.747
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.943
_reflns_number_gt                3708
_reflns_number_total             4800
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00149a2.cif
_cod_data_source_block           DICRO8Cu
_cod_depositor_comments
'Adding full bibliography for 7230120--7230121.cif.'
_cod_original_cell_volume        3012.3(9)
_cod_database_code               7230121
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.50(5)
 0.50(5)
2. Fixed Uiso
 At 1.2 times of:
  All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(Cr1) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O3A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Others
 Fixed Sof: Cr1(0.5) O3A(0.5) O4(0.5) Cr1A(0.5) O3(0.5)
 Fixed Uiso: H2(1)
5.a Riding coordinates:
 N4(H4)
5.b Aromatic/amide H refined with riding coordinates:
 N2(H2)
5.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C5(H5A,H5B,H5C), C10(H10A,H10B,H10C), C8(H8A,H8B,H8C)
;
_olex2_submission_special_instructions 'No special instructions were received'