Constructing New Metal-Organic Frameworks with Complicated Ligands Generated from “One-Pot” In Situ Reactions
Kong, Xiang-Jing; He, Tao; Zhang, Yongzheng; Wu, Xue-Qian; Wang, Si-Nan; Xu, Ming-Ming; Si, Guang-Rui; Li, Jian-Rong Jeff; Chemical Science  (2019) –; doi:10.1039/C9SC00178F

data_1550665
_publ_section_title
;
 Constructing New Metal-Organic Frameworks with Complicated Ligands
 Generated from &#x201C;One-Pot&#x201D; In Situ Reactions
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC00178F
_journal_year                    2019
_chemical_formula_moiety         'C74 H78 Mn4 N10 O22, 3(C3 H7 N O)'
_chemical_formula_sum            'C83 H99 Mn4 N13 O25'
_chemical_formula_weight         1898.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-04 deposited with the CCDC.    2019-02-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.4640(10)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   10.08670(10)
_cell_length_b                   15.6900(2)
_cell_length_c                   15.2941(2)
_cell_measurement_reflns_used    24042
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.2600
_cell_measurement_theta_min      2.8490
_cell_volume                     2332.82(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -126.00  -2.00   0.50    0.50    --  -36.20 -39.00  55.00  248
  2  \w   -140.00 -16.00   0.50    0.50    -- -105.40  39.00-149.00  248
  3  \w   -195.00 -71.00   0.50    0.50    -- -105.40 -39.00  55.00  248
  4  \w    -84.00  39.00   0.50    0.50    --    5.00 -39.00  55.00  246
  5  \w    -71.00  53.00   0.50    0.50    --  -36.20  38.00 120.00  248
  6  \w    -71.00  53.00   0.50    0.50    --  -36.20  69.00 150.84  248
  7  \w    -71.00  53.00   0.50    0.50    --  -36.20  39.00-149.00  248
  8  \w    -71.00  53.00   0.50    0.50    --  -36.20  41.00 -44.73  248
  9  \w    -71.00  53.00   0.50    0.50    --  -36.20  72.00   6.45  248
 10  \w   -140.00 -16.00   0.50    0.50    -- -105.40  72.00 150.00  248
 11  \w   -140.00 -16.00   0.50    0.50    -- -105.40  72.00-120.00  248
 12  \w   -140.00 -16.00   0.50    0.50    -- -105.40  72.00  30.00  248
 13  \w   -140.00 -16.00   0.50    0.50    -- -105.40  72.00  90.00  248
 14  \w   -140.00 -16.00   0.50    0.50    -- -105.40  72.00 -60.00  248
 15  \w   -195.00 -71.00   0.50    0.50    -- -105.40 -19.00-180.00  248
 16  \w   -140.00 -16.00   0.50    0.50    -- -105.40  72.00-180.00  248
 17  \w   -195.00 -71.00   0.50    0.50    -- -105.40 -47.00   5.31  248
 18  \w   -140.00 -16.00   0.50    0.50    -- -105.40  72.00   0.00  248
 19  \w   -140.00 -16.00   0.50    0.50    -- -105.40  19.00  60.00  248
 20  \w   -140.00 -16.00   0.50    0.50    -- -105.40  19.00 120.00  248
 21  \w   -140.00 -16.00   0.50    0.50    -- -105.40  72.00 -90.00  248
 22  \w   -195.00 -16.00   0.50    0.50    -- -105.40   0.00-150.00  358
 23  \w   -140.00 -16.00   0.50    0.50    -- -105.40  72.00   0.00  248
 24  \w   -140.00 -16.00   0.50    0.50    -- -105.40  72.00  60.00  248
 25  \w   -140.00 -16.00   0.50    0.50    -- -105.40  72.00 120.00  248
 26  \w   -140.00 -16.00   0.50    0.50    -- -105.40  38.00 -60.00  248
 27  \w   -140.00 -16.00   0.50    0.50    -- -105.40  57.00 120.00  248
 28  \w   -140.00 -16.00   0.50    0.50    -- -105.40  72.00-150.00  248
 29  \w   -140.00 -16.00   0.50    0.50    -- -105.40  72.00 -30.00  248
 30  \w    -29.00  94.00   0.50    0.50    --    5.00  57.00-180.00  246
 31  \w   -126.00  -2.00   0.50    0.50    --  -36.20 -69.00 114.24  248
 32  \w   -126.00  -2.00   0.50    0.50    --  -36.20 -58.00 -79.83  248
 33  \w   -126.00  -2.00   0.50    0.50    --  -36.20 -52.00 -46.50  248
 34  \w   -126.00  -2.00   0.50    0.50    --  -36.20 -38.00 -30.00  248
 35  \w   -126.00  -2.00   0.50    0.50    --  -36.20 -58.00-160.23  248
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0356752000
_diffrn_orient_matrix_UB_12      0.0326757000
_diffrn_orient_matrix_UB_13      0.0859313000
_diffrn_orient_matrix_UB_21      0.1370768000
_diffrn_orient_matrix_UB_22      -0.0355587000
_diffrn_orient_matrix_UB_23      0.0587981000
_diffrn_orient_matrix_UB_31      0.0709561000
_diffrn_orient_matrix_UB_32      0.0855742000
_diffrn_orient_matrix_UB_33      -0.0083085000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            40263
_diffrn_reflns_point_group_measured_fraction_full 0.884
_diffrn_reflns_point_group_measured_fraction_max 0.884
_diffrn_reflns_theta_full        67.075
_diffrn_reflns_theta_max         67.075
_diffrn_reflns_theta_min         2.998
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    4.963
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81755
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.35c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             988
_refine_diff_density_max         1.002
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details
;
 Flack x determined using 2814 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.008(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         7367
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0464
_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^)+(0.1029P)^2^+1.0512P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1312
_refine_ls_wR_factor_ref         0.1321
_reflns_Friedel_coverage         0.701
_reflns_Friedel_fraction_full    0.759
_reflns_Friedel_fraction_max     0.759
_reflns_number_gt                7208
_reflns_number_total             7367
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc00178f2.cif
_cod_data_source_block           BUT-103
_cod_database_code               1550665
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Mn C N O'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N7-C41
 1.5 with sigma of 0.01
 C13-O13
 1.25 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C41) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(N7)
\\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
4. Others
 Fixed Sof: C13(0.5) H13(0.5) N7(0.5) C42(0.5) H42A(0.5) H42B(0.5) H42C(0.5)
 C41(0.5) H41A(0.5) H41B(0.5) H41C(0.5) O13(0.5)
5.a Rotating group:
 N2(H2A,H2B), N1(H1A,H1B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C22(H22), C6(H6), C20(H20), C8(H8), C10(H10), C11(H11), C17(H17),
 C33(H33), C23(H23), C26(H26), C14(H14), C0AA(H0AA), C28(H28), C25(H25),
 C40(H40), C35(H35), C31(H31), C13(H13)
5.c Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C38(H38A,H38B,H38C), C32(H32A,H32B,H32C), C29(H29A,H29B,
 H29C), C37(H37A,H37B,H37C), C36(H36A,H36B,H36C), C39(H39A,H39B,H39C), C30(H30A,
 H30B,H30C), C42(H42A,H42B,H42C), C41(H41A,H41B,H41C)
;
_shelx_res_checksum              26334
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.184
_oxdiff_exptl_absorpt_empirical_full_min 0.898