An insight into sensitive detection of metal ions using a novel cobalt MOF: single crystal, photoluminescence, and theoretical studies
Rana, Love Karan; Kaur, Prabhjyot; Maris, Thierry; Duong, Adam; CrystEngComm  (2022) –; doi:10.1039/D2CE00385F

data_7245183
_publ_section_title
;
 An insight into sensitive detection of metal ions using a novel cobalt
 MOF: single crystal, photoluminescence, and theoretical studies
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00385F
_journal_year                    2022
_chemical_formula_moiety         'C36.46 H36.92 N4.46 Ni O8, 2(C2 H6 O)'
_chemical_formula_sum            'C40.46 H48.91 N4.46 Ni O10'
_chemical_formula_weight         816.30
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-06-20
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.06.18 svn.r64d69d6c for OlexSys, GUI svn.r6354)
;
_audit_update_record
;
2021-12-12 deposited with the CCDC.	2022-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                100.052(6)
_cell_angle_beta                 114.832(8)
_cell_angle_gamma                92.202(6)
_cell_formula_units_Z            1
_cell_length_a                   9.7970(9)
_cell_length_b                   9.9620(7)
_cell_length_c                   11.1350(9)
_cell_measurement_reflns_used    3695
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72
_cell_measurement_theta_min      3
_cell_volume                     963.51(15)
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'oxford diffraction'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_unetI/netI     0.0540
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6830
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.468
_diffrn_reflns_theta_min         4.475
_exptl_absorpt_coefficient_mu    1.270
_exptl_absorpt_correction_T_max  0.910
_exptl_absorpt_correction_T_min  0.842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Light-green
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_description       block
_exptl_crystal_F_000             431
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.355
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         3695
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0551
_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^)+(0.0832P)^2^+0.8648P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1564
_refine_ls_wR_factor_ref         0.1642
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3163
_reflns_number_total             3695
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00385f2.cif
_cod_data_source_block           ni-tere-26n3_auto
_cod_database_code               7245183
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.889
_shelx_estimated_absorpt_t_min   0.745
_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, All O(H) groups
2. Restrained distances
 O1A-H1AA
 0.85 with sigma of 0.01
 O1-H1A
 0.85 with sigma of 0.01
 C17-H1A
 1.886813 with sigma of 0.02
 C17A-H1AA
 1.887893 with sigma of 0.02
 Ni1-H1AA
 2.601027 with sigma of 0.02
 Ni1-H1A
 2.596243 with sigma of 0.02
 O5-C20 \\sim O5A-C20A
 with sigma of 0.02
 C20-C21 \\sim C20A-C21A
 with sigma of 0.02
 O5-C21 \\sim O5A-C21A
 with sigma of 0.04
 Ni1-O1 \\sim Ni1-O1A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C17) = Uanis(C17A)
Uanis(N1) = Uanis(C1A)
Uanis(O5) = Uanis(O5A)
Uanis(O1A) = Uanis(O1)
4. Rigid body (RIGU) restrains
 O5, O5A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(C20A)=Sof(H20C)=Sof(H20D)=Sof(C21A)=Sof(H21D)=Sof(H21E)=Sof(H21F)=
 Sof(O5A)=Sof(H5AA)=1-FVAR(1)
 Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(O5)=
 Sof(H5A)=FVAR(1)
 Sof(C17)=Sof(H17)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C19)=Sof(H19A)=
 Sof(H19B)=Sof(H19C)=Sof(N1)=Sof(O1)=Sof(H1A)=1-FVAR(2)
 Sof(C17A)=Sof(H17A)=Sof(H17B)=Sof(O1A)=Sof(H1AA)=Sof(C1A)=Sof(H1AB)=Sof(H1AC)=
 Sof(H1AD)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C17A(H17A,H17B), C20(H20A,H20B), C20A(H20C,H20D)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C5(H5), C6(H6), C7(H7), C9(H9), C13(H13), C15(H15), C16(H16),
 C17(H17), N3(H3)
6.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C1A(H1AB,H1AC,H1AD), C21(H21A,H21B,
 H21C), C21A(H21D,H21E,H21F)
6.d Idealised tetrahedral OH refined as rotating group:
 O5(H5A), O5A(H5AA)
;
_shelx_res_checksum              4022
_shelx_hkl_checksum              31363
_olex2_submission_special_instructions 'No special instructions were received'