Novel mode of 2-fold interpenetration observed in a primitive cubic network of formula [Ni(1,2-bis(4-pyridyl)acetylene)2(Cr2O7)]n
Hayley S. Scott; Alankriti Bajpai; Kai-Jie Chen; Tony Pham; Brian Space; John J. Perry,IV; Michael J. Zaworotko; Chem.Commun. 51 (2015) 14832–; doi:10.1039/C5cc05866J

data_7117859
_publ_section_title
;
 Novel mode of 2-fold interpenetration observed in a primitive cubic
 network of formula [Ni(1,2-bis(4-pyridyl)acetylene)2(Cr2O7)]n
;
_journal_name_full               Chem.Commun.
_journal_page_first              14832
_journal_paper_doi               10.1039/C5cc05866J
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         '0.5(C48 H32 Cr4 N8 Ni2 O14)'
_chemical_formula_sum            'C24 H16 Cr2 N4 Ni O7'
_chemical_formula_weight         635.12
_space_group_crystal_system      orthorhombic
_space_group_IT_number           23
_space_group_name_Hall           'I 2 2'
_space_group_name_H-M_alt        'I 2 2 2'
_symmetry_space_group_name_Hall  'I 2 2'
_symmetry_space_group_name_H-M   'I 2 2 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-08-14
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-08-15 deposited with the CCDC.
2015-08-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.5465(9)
_cell_length_b                   15.9683(17)
_cell_length_c                   20.726(2)
_cell_measurement_reflns_used    966
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      38.09
_cell_measurement_theta_min      3.49
_cell_volume                     2828.5(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1475
_diffrn_reflns_av_unetI/netI     0.2272
_diffrn_reflns_laue_measured_fraction_full 0.994
_diffrn_reflns_laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            4201
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        50.489
_diffrn_reflns_theta_max         50.489
_diffrn_reflns_theta_min         3.494
_exptl_absorpt_coefficient_mu    7.403
_exptl_absorpt_correction_T_max  0.3175
_exptl_absorpt_correction_T_min  0.2135
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_description       Block
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.447
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.119
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.52(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         1489
_refine_ls_number_restraints     196
_refine_ls_restrained_S_all      0.958
_refine_ls_R_factor_all          0.1902
_refine_ls_R_factor_gt           0.0956
_refine_ls_shift/su_max          3.222
_refine_ls_shift/su_mean         0.020
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1285P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2040
_refine_ls_wR_factor_ref         0.2406
_reflns_Friedel_coverage         0.715
_reflns_friedel_fraction_full    0.998
_reflns_friedel_fraction_max     0.998
_reflns_number_gt                719
_reflns_number_total             1489
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc05866j2.cif
_cod_data_source_block           dicro
_cod_original_cell_volume        2828.6(5)
_cod_database_code               7117859
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.48(5) 0.52(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 N1-C4'
 2.4 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C4) = Uanis(C5) = Uanis(C1) = Uanis(C2)
Uanis(C4') = Uanis(C5') = Uanis(C1') = Uanis(C2')
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C4')=Sof(H4')=Sof(C2')=Sof(H2')=Sof(C1')=Sof(H1')=Sof(C5')=Sof(H5')=1-
 FVAR(1)
 Sof(C2)=Sof(H2)=Sof(C1)=Sof(H1)=Sof(C5)=Sof(H5)=Sof(C4)=Sof(H4)=FVAR(1)
7.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C1(H1), C5(H5), C4(H4), C4'(H4'), C9(H9), C10(H10), C11(H11),
 C12(H12), C2'(H2'), C1'(H1'), C5'(H5')
7.b Fitted hexagon refined as free rotating group:
 C3(C2,C1,N1,C5,C4)
;