Co(II) coordination polymers constructed from a bent chiral linker: influencing framework topology using co-ligands
Tay, Hui Min; Hua, Carol; CrystEngComm  (2020) –; doi:10.1039/D0CE01172J

data_7241252
_publ_section_title
;
 Co(II) coordination polymers constructed from a bent chiral linker:
 influencing framework topology using co-ligands
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE01172J
_journal_year                    2020
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C68 H60 Co2 N8 O12, C3 H7 N O'
_chemical_formula_sum            'C71 H67 Co2 N9 O13'
_chemical_formula_weight         1372.19
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-04-02
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-08-10 deposited with the CCDC.	2020-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                85.6720(10)
_cell_angle_beta                 82.6900(10)
_cell_angle_gamma                83.4170(10)
_cell_formula_units_Z            1
_cell_length_a                   9.2097(2)
_cell_length_b                   11.18360(10)
_cell_length_c                   17.09640(10)
_cell_measurement_reflns_used    29081
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.8980
_cell_measurement_theta_min      3.9650
_cell_volume                     1731.75(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            52918
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         77.609
_diffrn_reflns_theta_min         2.611
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.316
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61401
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.36a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_description       block
_exptl_crystal_F_000             714
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.373
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.008(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     860
_refine_ls_number_reflns         13600
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0685
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1210P)^2^+1.4104P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1871
_refine_ls_wR_factor_ref         0.1913
_reflns_Friedel_coverage         0.896
_reflns_Friedel_fraction_full    0.950
_reflns_Friedel_fraction_max     0.871
_reflns_number_gt                12608
_reflns_number_total             13600
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01172j2.cif
_cod_data_source_block           compound_2_R
_cod_database_code               7241252
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C4) = Uanis(C0AA) = Uanis(C19) = Uanis(C1AA) = Uanis(C02C) = Uanis(C02B)
= Uanis(C01Q) = Uanis(C023)
Uanis(C02L) = Uanis(C02K) = Uanis(C6) = Uanis(C02J) = Uanis(C025) = Uanis(C01T)
Uanis(C2) = Uanis(C1) = Uanis(C9) = Uanis(C5) = Uanis(C3) = Uanis(C2AA)
Uanis(C13) = Uanis(C7AA) = Uanis(C9AA) = Uanis(C10) = Uanis(C0BA) = Uanis(C20)
Uanis(C01K) = Uanis(C02G) = Uanis(C022) = Uanis(C01P) = Uanis(C013) =
Uanis(C00Z)
Uanis(C02F) = Uanis(C12) = Uanis(C8)
Uanis(C3AA) = Uanis(C5AA) = Uanis(C01F)
Uanis(C10) = Uanis(C00S)
Uanis(C4AA) = Uanis(N1) = Uanis(N01L) = Uanis(C02H) = Uanis(C020) = Uanis(C7) =
Uanis(C01I) = Uanis(C3AA) = Uanis(C01Y) = Uanis(C5AA) = Uanis(C01F) =
Uanis(C016) = Uanis(C029) = Uanis(C14)
3. Others
 Sof(C01Q)=Sof(H01Q)=Sof(C023)=Sof(H023)=Sof(C02B)=Sof(H02G)=Sof(C02C)=
 Sof(H02H)=1-FVAR(1)
 Sof(C4)=Sof(H4)=Sof(C0AA)=Sof(H0AA)=Sof(C19)=Sof(H19)=Sof(C1AA)=Sof(H1AA)=
 FVAR(1)
 Sof(C00Z)=Sof(H00Z)=Sof(C013)=Sof(H013)=Sof(C01I)=Sof(H01I)=Sof(O01J)=
 Sof(C01K)=Sof(N01L)=Sof(H01L)=Sof(C01P)=Sof(C01T)=Sof(H01T)=Sof(C01Y)=
 Sof(H01Y)=Sof(C020)=Sof(C022)=Sof(H022)=Sof(C025)=Sof(H02C)=Sof(H02D)=
 Sof(C029)=Sof(H029)=Sof(O02A)=Sof(C02D)=Sof(C02G)=Sof(H02K)=Sof(C02H)=
 Sof(N02I)=Sof(H02L)=Sof(C02J)=Sof(H02M)=Sof(H02N)=Sof(C02K)=Sof(H02O)=
 Sof(H02P)=Sof(C02L)=Sof(H02Q)=Sof(C6)=Sof(H6A)=Sof(H6B)=1-FVAR(2)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C2AA)=
 Sof(H2AA)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(C3AA)=
 Sof(H3AA)=Sof(C7)=Sof(C14)=Sof(H14)=Sof(N1)=Sof(H1)=Sof(O2)=Sof(C4AA)=Sof(O1)=
 Sof(N2)=Sof(H2A)=Sof(C7AA)=Sof(H7AA)=Sof(C10)=Sof(C6AA)=Sof(C13)=Sof(C20)=
 Sof(H20)=Sof(C0BA)=Sof(H0BA)=Sof(C9AA)=Sof(H9AA)=Sof(C5AA)=Sof(H5AA)=FVAR(2)
 Fixed Sof: O00H(0.5) O00O(0.5) O0AA(0.5) O1AA(0.5)
4.a Ternary CH refined with riding coordinates:
 C01A(H01A), C01O(H01O), C01T(H01T), C02L(H02Q), C2(H2), C2AA(H2AA)
4.b Secondary CH2 refined with riding coordinates:
 C01H(H01D,H01F), C024(H02A,H02B), C025(H02C,H02D), C027(H02E,H02F), C02E(H02I,
 H02J), C02J(H02M,H02N), C02K(H02O,H02P), C6(H6A,H6B), C1(H1A,H1B), C3(H3A,H3B),
  C5(H5A,H5B), C9(H9A,H9B)
4.c Aromatic/amide H refined with riding coordinates:
 N008(H008), C00C(H00C), C00E(H00E), C00G(H00G), C00J(H00J), C00K(H00K),
 C00M(H00M), C00N(H00N), C00Q(H00Q), N00R(H00R), C00V(H00V), C00X(H00X),
 C00Y(H00Y), C00Z(H00Z), C012(H012), C013(H013), C014(H014), C016(H016),
 C017(H017), C018(H018), C019(H019), C01B(H01B), C01C(H01C), C01E(H01E),
 C01G(H01G), C01I(H01I), N01L(H01L), C01Q(H01Q), C01R(H01R), C01U(H01U),
 C01Y(H01Y), C01Z(H01Z), C022(H022), C023(H023), C028(H028), C029(H029),
 C02B(H02G), C02C(H02H), C02F(H02R), C02G(H02K), N02I(H02L), C4(H4), C0AA(H0AA),
  C19(H19), C1AA(H1AA), C3AA(H3AA), C14(H14), N1(H1), N2(H2A), C7AA(H7AA),
 C20(H20), C0BA(H0BA), C9AA(H9AA), C5AA(H5AA)
4.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C12(H12A,H12B,H12C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              29324
_shelx_fab_checksum              57082
_olex2_submission_special_instructions 'No special instructions were received'