Combination effect of ligand and ionic liquid components on the structure and property in manganese metal‒organic frameworks
Wei, Zhen; Zhang, Zong-Hui; Wang, Meng Meng; xu, ling; Liu, Bing; Jiao, Huan; CrystEngComm  (2017) –; doi:10.1039/C7CE01216K

data_7228876
_publ_section_title
;
 Combination effect of ligand and ionic liquid components on the structure
 and property in manganese metal--organic frameworks
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE01216K
_journal_year                    2017
_chemical_formula_moiety         '0.5(C84 H60 Mn4 O30), C7 H7 N3, C6 H8 N3'
_chemical_formula_sum            'C55 H45 Mn2 N6 O15'
_chemical_formula_weight         1139.85
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc1p9mk5
_audit_creation_date             2017-06-20
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2017-06-26 deposited with the CCDC.
2017-08-08 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 118.757(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.1886(10)
_cell_length_b                   21.2528(9)
_cell_length_c                   16.2865(7)
_cell_measurement_reflns_used    5643
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.4830
_cell_measurement_theta_min      3.4880
_cell_volume                     5519.2(5)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2002)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2002)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2002)'
_computing_molecular_graphics    'Siemens SHELXTL^TM^ 5'
_computing_publication_material  'Siemens SHELXTL^TM^ 5'
_computing_structure_refinement  'Siemens SHELXTL^TM^ 5'
_computing_structure_solution    'Siemens SHELXTL^TM^ 5'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            26303
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         4.09
_diffrn_source                   'rotating-anode generator'
_exptl_absorpt_coefficient_mu    0.529
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95694
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sphere (CrystalClear)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2348
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.045
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         4974
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0985
_refine_ls_R_factor_gt           0.0783
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1521P)^2^+11.0514P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2078
_refine_ls_wR_factor_ref         0.2294
_reflns_number_gt                3790
_reflns_number_total             4974
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7ce01216k2.cif
_cod_data_source_block           12
_cod_database_code               7228876
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C46-C47
 1.5 with sigma of 0.02
3. Rigid bond restraints
 N1, C1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
 N1, C4
 with sigma for 1-2 distances of 0.006 and sigma for 1-3 distances of 0.003
 N41, C44
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 N42, C41
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 C45, C46
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 C46, C47
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 N42, C45
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
Uanis(N1) \\sim Ueq, Uanis(N41) \\sim Ueq, Uanis(N42) \\sim Ueq, Uanis(C41)
\\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C46) \\sim Ueq,
Uanis(C47) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.005
5. Others
 Fixed Sof: H6a(0.5) H6b(0.5) H7a(0.5) H7b(0.5) H7c(0.5) H45a(0.5) H45b(0.5)
 H46a(0.5) H46b(0.5)
6.a Rotating group:
 O1W(H1Wa,H1Wb), O2W(H2W)
6.b Secondary CH2 refined with riding coordinates:
 C6(H6a,H6b), C44(H44a,H44b), C45(H45a,H45b), C46(H46a,H46b)
6.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C15(H15), C16(H16), C22(H22), C23(H23), C25(H25),
 C26(H26), C32(H32), C33(H33), C35(H35), C36(H36), C1(H1), C41(H41)
6.d Idealised Me refined as rotating group:
 C7(H7a,H7b,H7c)
;
_olex2_submission_special_instructions 'No special instructions were received'