A NbO type Cu(II) metal‒organic framework showing efficient catalytic activity in Friedländer and Henry reactions
Gupta, Anoop K.; De, Dinesh; Bharadwaj, Parimal K.; Dalton Trans.  (2017) –; doi:10.1039/C7DT01595J

data_7043151
_publ_section_title
;
 A NbO type Cu(II) metal--organic framework showing efficient catalytic
 activity in Friedl\"ander and Henry reactions
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01595J
_journal_year                    2017
_chemical_formula_moiety         '0.06(C180 H126 Cu18 N18 O90)'
_chemical_formula_sum            'C10 H7 Cu N O5'
_chemical_formula_weight         284.71
_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_Hall           '-R 3 2"'
_space_group_name_H-M_alt        'R -3 m'
_symmetry_space_group_name_Hall  '-R 3 2"'
_symmetry_space_group_name_H-M   'R -3 m :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-05-18
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r3563)
;
_audit_update_record
;
2017-05-26 deposited with the CCDC.
2017-05-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   18.604(5)
_cell_length_b                   18.604(5)
_cell_length_c                   37.123(5)
_cell_measurement_reflns_used    7626
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.46
_cell_measurement_theta_min      2.53
_cell_volume                     11127(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1756
_diffrn_reflns_av_unetI/netI     0.0747
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            41802
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         2.533
_exptl_absorpt_coefficient_mu    0.887
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5936
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0770 before and 0.0627 after correction.
The Ratio of minimum to maximum transmission is 0.7960.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    0.765
_exptl_crystal_description       Block
_exptl_crystal_F_000             2574
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.17
_platon_squeeze_details
;
TITL 30janc in R -3
CELL   18.6040   18.6040   37.1230     90.00     90.00    120.00
SPGR R-3m
C101 1.001 1.005 0.390 !       3.37 eA-3
C102 0.062 0.940 0.211 !       2.21 eA-3
C103 1.000 0.998 0.289 !       2.16 eA-3
Q104 0.951 0.470 0.001 !       2.00 eA-3
C105 0.309 0.153 0.398 !       1.93 eA-3
C106 0.971 0.481 0.735 !       1.90 eA-3
C107 0.234 0.748 0.080 !       1.87 eA-3
C108 0.668 0.332 0.916 !       1.86 eA-3
C109 1.001 0.998 0.265 !       1.86 eA-3
C110 0.999 1.005 0.367 !       1.83 eA-3
C111 0.625 0.247 0.100 !       1.82 eA-3
C112 0.127 0.876 0.194 !       1.77 eA-3
C113 1.000 1.005 0.219 !       1.74 eA-3
C114 0.284 0.138 0.813 !       1.73 eA-3
Q115 0.078 0.545 0.053 !       1.65 eA-3
C116 0.770 0.106 0.397 !       1.61 eA-3
C117 0.230 0.894 0.603 !       1.61 eA-3
Q118 0.265 0.128 0.611 !       1.59 eA-3
Q119 0.860 0.128 0.611 !       1.58 eA-3
Q120 0.844 0.701 0.609 !       1.48 eA-3
C121 0.626 0.308 0.093 !       1.46 eA-3
C122 0.300 0.214 0.958 !       1.46 eA-3
C123 0.380 0.184 0.547 !       1.40 eA-3
C124 0.809 0.184 0.548 !       1.40 eA-3
C125 0.609 0.384 0.149 !       1.38 eA-3
C126 1.000 0.998 0.242 !       1.38 eA-3
C127 0.812 0.904 0.133 !       1.32 eA-3
C128 0.049 0.954 0.108 !       1.31 eA-3
C129 0.176 0.424 0.493 !       1.30 eA-3
C130 0.782 0.889 0.155 !       1.27 eA-3
C131 0.454 0.028 0.742 !       1.27 eA-3
C132 0.866 0.215 0.390 !       1.26 eA-3
C133 0.859 0.731 0.781 !       1.26 eA-3
C134 0.736 0.606 0.384 !       1.25 eA-3
C135 0.231 0.762 0.486 !       1.23 eA-3
Q136 0.502 0.503 0.132 !       1.21 eA-3
C137 0.889 0.451 0.178 !       1.21 eA-3
C138 0.874 0.634 0.925 !       1.18 eA-3
C139 0.689 0.315 0.429 !       1.16 eA-3
C140 0.562 0.078 0.296 !       1.16 eA-3
C141 0.999 0.998 0.446 !       1.16 eA-3
C142 0.478 0.928 0.251 !       1.15 eA-3
C143 0.949 0.030 0.800 !       1.15 eA-3
C144 0.640 0.281 0.413 !       1.12 eA-3
C145 0.809 0.589 0.917 !       1.11 eA-3
Q146 0.815 0.108 0.619 !       1.11 eA-3
C147 0.757 0.566 0.920 !       1.10 eA-3
C148 0.579 0.418 0.132 !       1.09 eA-3
C149 0.826 0.441 0.216 !       1.08 eA-3
C150 0.302 0.702 0.052 !       1.08 eA-3
C151 1.000 0.994 0.016 !       1.06 eA-3
C152 0.736 0.514 0.304 !       1.06 eA-3
C153 0.235 0.497 0.556 !       1.06 eA-3
C154 0.497 0.762 0.554 !       1.06 eA-3
Q155 0.749 0.906 0.343 !       1.04 eA-3
C156 0.153 0.102 0.882 !       1.02 eA-3
C157 0.091 0.896 0.212 !       1.02 eA-3
C158 0.232 0.125 0.006 !       1.01 eA-3
C159 0.973 0.947 0.906 !       1.01 eA-3
Q160 0.595 0.793 0.227 !       1.00 eA-3
C161 0.796 0.449 0.234 !       0.98 eA-3
Q162 0.782 0.707 0.380 !       0.97 eA-3
C163 0.375 0.124 0.814 !       0.97 eA-3
C164 0.370 0.629 0.252 !       0.97 eA-3
C165 0.887 0.016 0.899 !       0.97 eA-3
C166 0.904 0.421 0.190 !       0.96 eA-3
C167 0.971 0.032 0.007 !       0.95 eA-3
C168 0.784 0.395 0.375 !       0.95 eA-3
C169 0.142 0.276 0.484 !       0.95 eA-3
C170 0.174 0.658 0.757 !       0.94 eA-3
C171 0.941 0.893 0.399 !       0.94 eA-3
C172 0.985 0.012 0.195 !       0.94 eA-3
C173 0.127 0.037 0.088 !       0.93 eA-3
C174 0.094 0.550 0.672 !       0.93 eA-3
C175 0.112 0.062 0.015 !       0.92 eA-3
C176 1.000 1.000 0.500 !       0.92 eA-3
C177 0.109 0.392 0.149 !       0.92 eA-3
C178 0.439 0.566 0.202 !       0.91 eA-3
C179 0.534 0.543 0.140 !       0.91 eA-3
C180 0.704 0.299 0.476 !       0.91 eA-3
C181 0.341 0.227 0.421 !       0.89 eA-3
C182 0.593 0.609 0.256 !       0.89 eA-3
C183 0.030 0.763 0.468 !       0.89 eA-3
C184 0.970 0.237 0.532 !       0.89 eA-3
Q185 0.189 0.091 0.610 !       0.89 eA-3
C186 0.092 0.542 0.891 !       0.89 eA-3
Q187 0.640 0.557 0.869 !       0.88 eA-3
C188 0.089 0.056 0.742 !       0.88 eA-3
C189 0.455 0.959 0.827 !       0.87 eA-3
C190 0.812 0.449 0.132 !       0.86 eA-3
C191 0.722 0.746 0.494 !       0.86 eA-3
C192 0.171 0.191 0.063 !       0.86 eA-3
Q193 0.922 0.847 0.584 !       0.86 eA-3
C194 0.811 0.184 0.821 !       0.86 eA-3
C195 0.298 0.695 0.312 !       0.86 eA-3
C196 0.498 0.956 0.827 !       0.86 eA-3
Q197 0.158 0.846 0.788 !       0.85 eA-3
C198 0.330 0.671 0.772 !       0.85 eA-3
C199 0.313 0.623 0.111 !       0.84 eA-3
;
_refine_diff_density_max         1.331
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         2543
_refine_ls_number_restraints     116
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.1557
_refine_ls_R_factor_gt           0.0915
_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^)+(0.1698P)^2^+34.9172P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2509
_refine_ls_wR_factor_ref         0.2959
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1450
_reflns_number_total             2543
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01595j2.cif
_cod_data_source_block           30janc_sq
_cod_original_cell_volume        11127(6)
_cod_database_code               7043151
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.864
_shelx_estimated_absorpt_t_min   0.789
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 N1B-N1A
 0.6 with sigma of 0.02
 C6B-C6A
 0.7 with sigma of 0.02
 N1B-C5 \\sim N1A-C5
 with sigma of 0.001
 N1A-C6B \\sim N1B-C6A
 with sigma of 0.001
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C6A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C6B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C4, Cu1, O2, O3, OW1, C1, C2, C3, C5, N1B, C6A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C6A, N1B, C5, C4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C4, C5, N1A, C6B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Fixed Sof: N1B(0.25) C6B(0.5) H6BA(0.5) H6BB(0.5) N1A(0.25) C6A(0.5)
 H6AA(0.5) H6AB(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C6B(H6BA,H6BB), C6A(H6AA,H6AB)
7.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3)
;
_shelx_res_checksum              23432
_shelx_fab_checksum              29762
_olex2_submission_special_instructions 'No special instructions were received'