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_7230120
_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         'C20 H22 Cr2 Cu N6 O7'
_chemical_formula_sum            'C20 H22 Cr2 Cu N6 O7'
_chemical_formula_weight         625.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-01-08
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2018-01-10 deposited with the CCDC.
2018-02-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.47(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.710(3)
_cell_length_b                   14.320(3)
_cell_length_c                   15.800(3)
_cell_measurement_reflns_used    36754
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      27.499
_cell_measurement_theta_min      1.393
_cell_volume                     3307.0(12)
_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 0.999
_diffrn_measurement_device_type  'Australian Synchrotron'
_diffrn_measurement_method       'scans in phi'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0774
_diffrn_reflns_av_unetI/netI     0.0600
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            36754
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         1.393
_exptl_absorpt_coefficient_mu    1.322
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XSCALE in XDS'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_description       block
_exptl_crystal_F_000             1268
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.998
_refine_diff_density_min         -0.897
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         7598
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0517
_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^)+(0.0637P)^2^+3.3087P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1457
_refine_ls_wR_factor_ref         0.1482
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6898
_reflns_number_total             7598
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00149a2.cif
_cod_data_source_block           DICRO7Cu
_cod_depositor_comments
'Adding full bibliography for 7230120--7230121.cif.'
_cod_database_code               7230120
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.974
_shelx_estimated_absorpt_t_min   0.949
_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
2. Restrained distances
 N3-H3
 0.86 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O5) \\sim Ueq, Uanis(O6) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.01
4. Others
 Fixed Sof: Cr2A(0.5) O6A(0.5) Cr2(0.5) O6(0.5) O5A(0.5) O5(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C15(H15), C14(H14), N6(H6), C12(H12), N3(H3), C11(H11), C1(H1), C2(H2),
 C4(H4), C5(H5)
5.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C18(H18A,H18B,H18C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C)
;
_olex2_submission_special_instructions 'No special instructions were received'