Solvent-Directed Control over the Topology of Entanglement in Square Lattice (sql) Coordination Networks
Zaworotko, Michael; Sanii, Rana; Hua, Carol; Patyk-Kaźmierczak, Ewa; Chemical Communications  (2019) –; doi:10.1039/C8CC09152H

data_7122781
_publ_section_title
;
 Solvent-Directed Control over the Topology of Entanglement in Square
 Lattice (sql) Coordination Networks
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC09152H
_journal_year                    2019
_chemical_formula_moiety         'C104 H80 Co2 N28 O12, H2 O'
_chemical_formula_sum            'C104 H82 Co2 N28 O13'
_chemical_formula_weight         2049.83
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-06-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;
_audit_update_record
;
2018-11-05 deposited with the CCDC.
2019-01-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.0586(9)
_cell_length_b                   9.5030(4)
_cell_length_c                   44.7513(18)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.96
_cell_measurement_theta_min      2.81
_cell_volume                     9380.9(7)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.97
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_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  0.0548
_diffrn_reflns_av_unetI/netI     0.0458
_diffrn_reflns_Laue_measured_fraction_full 0.956
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            33926
_diffrn_reflns_point_group_measured_fraction_full 0.956
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        60.985
_diffrn_reflns_theta_max         60.985
_diffrn_reflns_theta_min         1.974
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.454
_exptl_absorpt_correction_T_max  0.7529
_exptl_absorpt_correction_T_min  0.6411
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0816 before and 0.0693 after correction. The Ratio of minimum to maximum transmission is 0.8515. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_description       needle
_exptl_crystal_F_000             4240
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.763
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     692
_refine_ls_number_reflns         6863
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.0933
_refine_ls_R_factor_gt           0.0752
_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^)+(0.0390P)^2^+45.1361P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1651
_refine_ls_wR_factor_ref         0.1732
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5560
_reflns_number_total             6863
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc09152h2.cif
_cod_data_source_block           comp1
_cod_database_code               7122781
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.903
_shelx_estimated_absorpt_t_min   0.662
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O3E-O4E = O4E-O1E = O3E-O1E
 2.2 with sigma of 0.02
 N2E-O1E = N2E-O4E = N2E-O3E
 1.2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O1E \\sim O3E \\sim O4E \\sim N2E: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
O1D \\sim O3D \\sim O4D \\sim N2D: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Sof(O1E)=Sof(O3E)=Sof(O4E)=Sof(N2E)=1-FVAR(1)
 Sof(O1D)=Sof(O3D)=Sof(O4D)=Sof(N2D)=FVAR(1)
 Fixed Sof: O1F(0.5) H1FA(0.5) H1FB(0.5)
5.a Riding coordinates:
 O1F(H1FA,H1FB)
5.b Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C2B(H2B), C4A(H4A), C4B(H4B), C5A(H5A), C5B(H5B), C7A(H7A),
 C7B(H7B), C8A(H8A), C8B(H8B), C10A(H10A), C10B(H10B), C11A(H11A), C11B(H11B),
 C13A(H13A), C13B(H13B), C15A(H15A), C15B(H15B), C16A(H16A), C16B(H16B),
 C18A(H18A), C18B(H18B), C19A(H19A), C19B(H19B), C20A(H20A), C20B(H20B),
 C27A(H27A), C26A(H26A), C24A(H24A), C23A(H23A), C23B(H23B), C24B(H24B),
 C26B(H26B), C27B(H27B), C29A(H29A), C29B(H29B), C31A(H31A), C31B(H31B),
 C32A(H32A), C32B(H32B)
5.c Fitted hexagon refined as free rotating group:
 C22A(C27A,C26A,C25A,C24A,C23A)
;
_shelx_res_checksum              74055
_shelx_hkl_checksum              60904
_olex2_submission_special_instructions 'No special instructions were received'