Tuning of the flexibility in metal-organic frameworks based on pendant arm macrocycles
Jeoung, Sungeun; Lee, Songho; Lee, Jae Hwa; Lee, Soochan; Choe, Wonyoung; Moon, Dohyun; Moon, Hoi Ri; Chemical Communications  (2019) –; doi:10.1039/C9CC02819F

data_7123542
_publ_section_title
;
 Tuning of the flexibility in metal-organic frameworks based on pendant
 arm macrocycles
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC02819F
_journal_year                    2019
_chemical_formula_moiety         'C44 H66 N12 Ni2 O8, 2(C2 H3 N)'
_chemical_formula_sum            'C48 H72 N14 Ni2 O8'
_chemical_formula_weight         1090.61
_chemical_name_systematic        as-flexMOF(CH2)
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-05-17 deposited with the CCDC.    2019-05-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.16(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.920(3)
_cell_length_b                   32.634(7)
_cell_length_c                   15.617(3)
_cell_measurement_reflns_used    92121
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      33.679
_cell_measurement_theta_min      0.350
_cell_volume                     6355(3)
_computing_cell_refinement       '<i>HKL3000sm</i>(Otwinowski & Minor, 1997)'
_computing_data_collection
'<i>PAL BL2D-SMDC Program</i>(Shin et.al, 2016)'
_computing_data_reduction        '<i>HKL3000sm</i>(Otwinowski & Minor, 1997)'
_computing_molecular_graphics    '<i>DIAMOND 4</i>(Putz&Brandenburg, 2014)'
_computing_publication_material  '<i>publCIF</i>(Westrip, 2010)'
_computing_structure_refinement  '<i>SHELXL-2018</i>(Sheldrick, 2015b)'
_computing_structure_solution    '<i>SHELXT-2018</i>(Sheldrick, 2015a)'
_diffrn_ambient_temperature      220(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.610
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31733
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        21.469
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.500
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    0.428
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.918
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'<i>HKL3000sm Scalepack</i>(Otwinowski et.al,2003)'
_exptl_crystal_colour            'pale purple'
_exptl_crystal_density_diffrn    1.140
_exptl_crystal_description       block
_exptl_crystal_F_000             2312
_exptl_crystal_size_max          0.215
_exptl_crystal_size_mid          0.198
_exptl_crystal_size_min          0.105
_refine_diff_density_max         1.270
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       0.0024(8)
_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   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         8742
_refine_ls_number_restraints     296
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0784
_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^)+(0.1896P)^2^+1.3860P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2657
_refine_ls_wR_factor_ref         0.2778
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6808
_reflns_number_total             8742
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc02819f2.cif
_cod_data_source_block           asflex_CH2_sq
_cod_original_cell_volume        6355(2)
_cod_database_code               7123542
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.914
_shelx_estimated_absorpt_t_max   0.956
_shelx_res_checksum              76826
_shelx_fab_checksum              43304