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_7245185
_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         'C138 H94 N6 O30 Zn8, 4(C3 H7 N O)'
_chemical_formula_sum            'C150 H122 N10 O34 Zn8'
_chemical_formula_weight         3131.53
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2021-12-21 deposited with the CCDC.	2022-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.7360(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.2418(9)
_cell_length_b                   26.6132(9)
_cell_length_c                   31.8614(10)
_cell_measurement_reflns_used    9956
_cell_measurement_temperature    150
_cell_measurement_theta_max      60.752
_cell_measurement_theta_min      3.169
_cell_volume                     21456.9(12)
_computing_cell_refinement
;
SAINT (2013) V8.38A; Integration Software for Single Crystal Data.
Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_data_collection
'APEX 2 (2013) Bruker AXS Inc., Madison, WI 53719-1173.'
_computing_data_reduction
;
SAINT (2013) V8.38A; Integration Software for Single Crystal Data.
Bruker AXS Inc., Madison, WI 53719-1173.
;
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'CMOS Area detector'
_diffrn_detector_area_resol_mean 10.24
_diffrn_detector_type            'Bruker Photon 100 CMOS Detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker Venture Metaljet'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_collimation    'Focusing mirrors'
_diffrn_radiation_monochromator  'Helios MX Mirror Optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            291945
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         60.826
_diffrn_reflns_theta_min         2.096
_diffrn_source                   'Metal Jet'
_diffrn_source_target            Ga
_diffrn_source_type              'Gallium Liquid Metal Jet Source'
_exptl_absorpt_coefficient_mu    0.931
_exptl_absorpt_correction_T_max  0.7519
_exptl_absorpt_correction_T_min  0.6830
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0785 before and 0.0560 after correction.
The Ratio of minimum to maximum transmission is 0.9084.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.969
_exptl_crystal_description       Block
_exptl_crystal_F_000             6416
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.32
_refine_diff_density_max         1.527
_refine_diff_density_min         -1.059
_refine_diff_density_rms         0.103
_refine_ls_extinction_coef       0.00097(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1715
_refine_ls_number_reflns         49420
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0578
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1175P)^2^+17.5755P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1826
_refine_ls_wR_factor_ref         0.1880
_reflns_Friedel_coverage         0.000
_reflns_number_gt                43125
_reflns_number_total             49420
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00385f2.cif
_cod_data_source_block           ada193_sq
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               7245185
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.755
_shelx_estimated_absorpt_t_min   0.719
_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. Restrained distances
 N5-C134 \\sim N5-C135 \\sim C136-N6A \\sim C139-N6B \\sim N6A-C137 \\sim
N6A-C138 \\sim N6B-C140 ~
 N6B-C141
 with sigma of 0.002
 Zn8-O19A \\sim Zn8-O19B
 with sigma of 0.02
 O19A-C136 \\sim O19B-C139
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O1C \\sim C1C \\sim N1C \\sim C2C \\sim C3C: within 1.7A with sigma of 0.002
and sigma for terminal atoms of 0.02 within 1.7A
O19A \\sim C137 \\sim N6A \\sim C137 \\sim C138 \\sim O19B \\sim C139 \\sim N6B
\\sim C140 \\sim N6B \\sim C141: within 1.7A with sigma of 0.002 and sigma for
terminal atoms of 0.02 within 1.7A
4. Others
 Fixed Sof: O19A(0.5) C136(0.5) H136(0.5) N6A(0.5) C137(0.5) H13G(0.5)
 H13H(0.5) H13I(0.5) C138(0.5) H13J(0.5) H13K(0.5) H13L(0.5) O19B(0.5)
 C139(0.5) H139(0.5) N6B(0.5) C140(0.5) H14A(0.5) H14B(0.5) H14C(0.5) C141(0.5)
 H14D(0.5) H14E(0.5) H14F(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C114(H11A,H11B), C127(H12A,H12B)
5.b Me refined with riding coordinates:
 C134(H13A,H13B,H13C), C135(H13D,H13E,H13F), C137(H13G,H13H,H13I), C138(H13J,
 H13K,H13L), C140(H14A,H14B,H14C), C141(H14D,H14E,H14F), C2A(H2AA,H2AB,H2AC),
 C1A(H1AA,H1AB,H1AC), C1D(H1DA,H1DB,H1DC), C3B(H3BA,H3BB,H3BC), C2C(H2CA,H2CB,
 H2CC), C3C(H3CA,H3CB,H3CC), C2D(H2DA,H2DB,H2DC), C3D(H3DA,H3DB,H3DC)
5.c Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3), C3(H3A), C4(H4), C6(H6), C7(H7), C9(H9), C11(H11), C13(H13),
 C15(H15), C16(H16), C18(H18), C19(H19), C22(H22), C23(H23), C25(H25), C26(H26),
  C30(H30), C31(H31), C33(H33), C34(H34), C36(H36), C38(H38), C40(H40),
 C42(H42), C43(H43), C45(H45), C46(H46), C49(H49), C50(H50), C52(H52), C53(H53),
  C57(H57), C58(H58), C60(H60), C61(H61), C63(H63), C65(H65), C67(H67),
 C69(H69), C70(H70), C72(H72), C73(H73), C76(H76), C77(H77), C79(H79), C80(H80),
  C84(H84), C85(H85), C87(H87), C88(H88), C90(H90), C92(H92), C94(H94),
 C96(H96), C97(H97), C99(H99), C100(H100), C103(H103), C104(H104), C106(H106),
 C107(H107), C109(H109), C110(H110), C111(H111), C113(H113), C117(H117),
 C119(H119), C120(H120), C122(H122), C124(H124), C125(H125), C129(H129),
 C130(H130), C131(H131), C132(H132), C133(H133), C136(H136), C139(H139),
 C1C(H1C), C2B(H2B), C1B(H1B), C1E(H1E)
;
_shelx_res_checksum              24529
_shelx_hkl_checksum              75984
_shelx_fab_checksum              31186
_platon_squeeze_special_details
;
A solvent mask was calculated and 1441 electrons were 
found in a volume of 9906\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
36[C3H7NO] per Unit Cell 
which account for 1440 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'