Structural Diversity, Gas Adsorption and Magnetic Property of Three Coordination Polymers based on Rigid Multicarboxylate Ligand
Gao, Lingling; Bian, Yongjun; Tian, Yuan; chen, yongqiang; Hu, Tuoping; CrystEngComm  (2020) –; doi:10.1039/D0CE01201G

data_7241304
_publ_section_title
;
 Structural Diversity, Gas Adsorption and Magnetic Property of Three
 Coordination Polymers based on Rigid Multicarboxylate Ligand
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE01201G
_journal_year                    2020
_chemical_formula_moiety         'C106 H73 Co6 N12 O22'
_chemical_formula_sum            'C106 H73 Co6 N12 O22'
_chemical_formula_weight         2220.34
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-11-12
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-02-24 deposited with the CCDC.	2020-09-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   33.5570(11)
_cell_length_b                   15.8380(5)
_cell_length_c                   20.0331(6)
_cell_measurement_reflns_used    9858
_cell_measurement_temperature    298.15
_cell_measurement_theta_max      25.17
_cell_measurement_theta_min      2.572
_cell_volume                     10647.1(6)
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1035
_diffrn_reflns_av_unetI/netI     0.0892
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            114929
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.462
_diffrn_reflns_theta_min         2.229
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.987
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6962
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0763 before and 0.0701 after correction. The Ratio of minimum to maximum transmission is 0.9340. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_description       block
_exptl_crystal_F_000             4523
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.614
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.27(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1479
_refine_ls_number_reflns         21258
_refine_ls_number_restraints     557
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.1131
_refine_ls_R_factor_gt           0.0544
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0729P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1178
_refine_ls_wR_factor_ref         0.1400
_reflns_Friedel_coverage         0.942
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                13523
_reflns_number_total             21258
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01201g2.cif
_cod_data_source_block           mo_1031_4_0ma_sq
_cod_database_code               7241304
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.827
_shelx_estimated_absorpt_t_min   0.756
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.73(2)
 0.27(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
3. Restrained distances
 C54A-C55A
 2.4 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C40) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C40A)
\\sim Ueq, Uanis(C41A) \\sim Ueq, Uanis(C42A) \\sim Ueq, Uanis(C43) \\sim Ueq,
Uanis(C44) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C47)
\\sim Ueq, Uanis(C46A) \\sim Ueq, Uanis(C45A) \\sim Ueq, Uanis(C44A) \\sim Ueq,
Uanis(C43A) \\sim Ueq, Uanis(C47A) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C49)
\\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C52) \\sim Ueq,
Uanis(C52A) \\sim Ueq, Uanis(C51A) \\sim Ueq, Uanis(C49A) \\sim Ueq,
Uanis(C48A) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C50A) \\sim Ueq, Uanis(C53A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N7) \\sim Ueq, Uanis(N8) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C55)
\\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(N7A) \\sim Ueq, Uanis(C54A) \\sim Ueq,
Uanis(C56A) \\sim Ueq, Uanis(C55A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C13) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C20)
\\sim Ueq, Uanis(C19) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
5. Rigid body (RIGU) restrains
 N6, N7, C40, C40A, C41, C41A, C42, C42A, C43, C43A, C44, C44A, C45, C45A, C46,
  C46A, C47, C47A, C48, C48A, C49, C49A, C50, C50A, C51, C51A, C52, C52A, C53,
 C53A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N7, N7A, N8, C53, C53A, C54, C54A, C55, C55A, C56, C56A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(N7A)=Sof(C40A)=Sof(H40C)=Sof(H40D)=Sof(C41A)=Sof(C42A)=Sof(H42A)=
 Sof(C43A)=Sof(H43A)=Sof(C44A)=Sof(C45A)=Sof(H45A)=Sof(C46A)=Sof(H46A)=
 Sof(C47A)=Sof(C48A)=Sof(H48A)=Sof(C49A)=Sof(H49A)=Sof(C50A)=Sof(C51A)=
 Sof(H51A)=Sof(C52A)=Sof(H52A)=Sof(C53A)=Sof(H53C)=Sof(H53D)=Sof(C54A)=
 Sof(H54A)=Sof(C55A)=Sof(H55A)=Sof(C56A)=Sof(H56A)=1-FVAR(1)
 Sof(N7)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(C41)=Sof(C42)=Sof(H42)=Sof(C43)=
 Sof(H43)=Sof(C44)=Sof(C45)=Sof(H45)=Sof(C46)=Sof(H46)=Sof(C47)=Sof(C48)=
 Sof(H48)=Sof(C49)=Sof(H49)=Sof(C50)=Sof(C51)=Sof(H51)=Sof(C52)=Sof(H52)=
 Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(C54)=Sof(H54)=Sof(C55)=Sof(H55)=Sof(C56)=
 Sof(H56)=FVAR(1)
7.a Ternary CH refined with riding coordinates:
 O4(H4)
7.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C17(H17A,H17B), C40(H40A,H40B), C40A(H40C,H40D), C53(H53A,
 H53B), C53A(H53C,H53D), C80(H80A,H80B), C93(H93A,H93B)
7.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C11(H11), C12(H12), C14(H14),
 C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C23(H23), C26(H26), C28(H28),
  C31(H31), C33(H33), C34(H34), C37(H37), C38(H38), C39(H39), C42(H42),
 C42A(H42A), C43(H43), C43A(H43A), C45(H45), C45A(H45A), C46(H46), C46A(H46A),
 C48(H48), C48A(H48A), C49(H49), C49A(H49A), C51(H51), C51A(H51A), C52(H52),
 C52A(H52A), C54(H54), C54A(H54A), C55(H55), C55A(H55A), C56(H56), C56A(H56A),
 C59(H59), C60(H60), C63(H63), C66(H66), C68(H68), C71(H71), C73(H73), C74(H74),
  C77(H77), C78(H78), C79(H79), C82(H82), C83(H83), C85(H85), C86(H86),
 C88(H88), C89(H89), C91(H91), C92(H92), C94(H94), C95(H95), C96(H96), C99(H99),
  C100(H100), C102(H102), C105(H105)
;
_shelx_res_checksum              26908
_shelx_fab_checksum              16133
_olex2_submission_special_instructions 'No special instructions were received'