An expanded MIL-53-type coordination polymer with a reactive pendant ligand
Kunicki, Hannah; Chamberlain, Thomas W.; Clarkson, Guy J.; Kashtiban, Reza J.; Hooper, Joseph E.; Dawson, Daniel M.; Ashbrook, Sharon E.; Walton, Richard I.; CrystEngComm 20 (2018) 4355–; doi:10.1039/C8CE00891D

data_7231207
_publ_section_title
;
 An expanded MIL-53-type coordination polymer with a reactive pendant
 ligand
;
_journal_issue                   31
_journal_name_full               CrystEngComm
_journal_page_first              4355
_journal_paper_doi               10.1039/C8CE00891D
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         '0.25(C216 H152 Mg8 N8 O40)'
_chemical_formula_sum            'C54 H38 Mg2 N2 O10'
_chemical_formula_weight         923.48
_space_group_crystal_system      orthorhombic
_space_group_IT_number           57
_space_group_name_Hall           '-P 2c 2b'
_space_group_name_H-M_alt        'P b c m'
_symmetry_space_group_name_Hall  '-P 2c 2b'
_symmetry_space_group_name_H-M   'P b c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-03-02
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3461 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-05-08 deposited with the CCDC.
2018-06-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.59874(19)
_cell_length_b                   7.14697(12)
_cell_length_c                   50.2201(8)
_cell_measurement_reflns_used    17368
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.2720
_cell_measurement_theta_min      5.3110
_cell_volume                     5957.65(15)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
'#__ type_ start__ end____ width___ exp.time_ 1 omega -107.00 73.00 0.5000 5.0000 omega____ theta____ kappa____ phi______ frames - -17.0000 40.0000 0.0000 360 #__ type_ start__ end____ width___ exp.time_ 2 omega -179.00 0.00 0.5000 28.0000 omega____ theta____ kappa____ phi______ frames - -90.0000 30.0000 120.0000 358 #__ type_ start__ end____ width___ exp.time_ 3 omega -162.00 -0.50 0.5000 28.0000 omega____ theta____ kappa____ phi______ frames - -90.0000 30.0000 -120.0000 323 #__ type_ start__ end____ width___ exp.time_ 4 omega -155.50 -18.00 0.5000 28.0000 omega____ theta____ kappa____ phi______ frames - -90.0000 60.0000 -60.0000 275 #__ type_ start__ end____ width___ exp.time_ 5 omega -122.00 -57.00 0.5000 28.0000 omega____ theta____ kappa____ phi______ frames - -90.0000 0.0000 30.0000 130 #__ type_ start__ end____ width___ exp.time_ 6 omega -156.00 -78.00 0.5000 28.0000 omega____ theta____ kappa____ phi______ frames - -90.0000 60.0000 30.0000 156 #__ type_ start__ end____ width___ exp.time_ 7 omega -115.00 -4.50 0.5000 28.0000 omega____ theta____ kappa____ phi______ frames - -90.0000 60.0000 90.0000 221 #__ type_ start__ end____ width___ exp.time_ 8 omega -142.50 -118.00 0.5000 28.0000 omega____ theta____ kappa____ phi______ frames - -90.0000 50.0000 60.0000 49 #__ type_ start__ end____ width___ exp.time_ 9 omega -179.00 -95.00 0.5000 28.0000 omega____ theta____ kappa____ phi______ frames - -90.0000 60.0000 -90.0000 168'
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0057083000
_diffrn_orient_matrix_UB_12      0.1548636000
_diffrn_orient_matrix_UB_13      -0.0212621000
_diffrn_orient_matrix_UB_21      0.0919363000
_diffrn_orient_matrix_UB_22      -0.0087926000
_diffrn_orient_matrix_UB_23      -0.0040237000
_diffrn_orient_matrix_UB_31      -0.0113924000
_diffrn_orient_matrix_UB_32      -0.1497014000
_diffrn_orient_matrix_UB_33      -0.0217390000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_unetI/netI     0.0120
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       59
_diffrn_reflns_limit_l_min       -60
_diffrn_reflns_number            44127
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.402
_diffrn_reflns_theta_max         67.402
_diffrn_reflns_theta_min         2.662
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.771
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78407
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.030
_exptl_crystal_description       block
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.126
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         5431
_refine_ls_number_restraints     248
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0772
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1390P)^2^+5.9147P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2424
_refine_ls_wR_factor_ref         0.2474
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4772
_reflns_number_total             5431
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00891d2.cif
_cod_data_source_block           hk4southamptonp_sq
_cod_depositor_comments
'Adding full bibliography for 7231205--7231207.cif.'
_cod_original_cell_volume        5957.64(15)
_cod_database_code               7231207
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C27 H28 Mg N O5'
_shelx_estimated_absorpt_t_max   0.955
_shelx_estimated_absorpt_t_min   0.831
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.29
_olex2_refinement_description
;
The Squeeze routine was used to model the contribution form disordered solvent

1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C8A-C9A = C5B-C8B = C8B-C9B = C9B-C10B
 1.35 with sigma of 0.02
 C9-C10C = C6-C5C = C12-C11C = C14C-C13C
 1.395 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O1B \\sim N2B \\sim C3B \\sim C4B \\sim C5B \\sim C6B \\sim C7B \\sim C8B \\sim
C9B \\sim C10B \\sim C11B \\sim C12B \\sim C13B \\sim C14B \\sim C15B: within
1.7A with sigma of 0.003 and sigma for terminal atoms of 0.006
O1A \\sim N2A \\sim C3A \\sim C4A \\sim C5A \\sim C6A \\sim C7A \\sim C8A \\sim
C9A \\sim C10A \\sim C11A \\sim C12A \\sim C13A \\sim C14A \\sim C15A: within
1.7A with sigma of 0.003 and sigma for terminal atoms of 0.006
C10C \\sim C11C \\sim C12 \\sim C13C \\sim C14C: within 1.7A with sigma of 0.01
and sigma for terminal atoms of 0.02
C3 \\sim C4C \\sim C5C \\sim C7C \\sim C8C: within 1.7A with sigma of 0.002 and
sigma for terminal atoms of 0.004
4. Others
 Sof(C4C)=Sof(H4C)=Sof(C5C)=Sof(H5C)=Sof(C8C)=Sof(H8C)=Sof(C7C)=Sof(H7C)=
 Sof(C10C)=Sof(H10C)=Sof(C13C)=Sof(H13C)=Sof(C11C)=Sof(H11C)=Sof(C14C)=
 Sof(H14C)=1-FVAR(1)
 Sof(C7)=Sof(H7)=Sof(C10)=Sof(H10)=Sof(C8)=Sof(H8)=Sof(C11)=Sof(H11)=Sof(C5)=
 Sof(H5)=Sof(C4)=Sof(H4)=Sof(C13)=Sof(H13)=Sof(C14)=Sof(H14)=FVAR(1)
 Fixed Sof: N2B(0.5) C3B(0.5) H3B(0.5) C4B(0.5) H4B(0.5) C5B(0.5) C6B(0.5)
 H6B(0.5) C7B(0.5) H7B(0.5) C8B(0.5) H8B(0.5) C9B(0.5) H9B(0.5) C10B(0.5)
 C11B(0.5) H11B(0.5) C12B(0.5) H12B(0.5) C13B(0.5) H13B(0.5) C14B(0.5)
 H14B(0.5) C15B(0.5) H15B(0.5) N2A(0.5) C3A(0.5) H3A(0.5) C4A(0.5) H4A(0.5)
 C5A(0.5) C6A(0.5) H6A(0.5) C7A(0.5) H7A(0.5) C8A(0.5) H8A(0.5) C9A(0.5)
 H9A(0.5) C10A(0.5) C11A(0.5) H11A(0.5) C12A(0.5) H12A(0.5) C13A(0.5) H13A(0.5)
 C14A(0.5) H14A(0.5) C15A(0.5) H15A(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C3B(H3B), C4B(H4B), C6B(H6B), C7B(H7B), C8B(H8B), C9B(H9B), C11B(H11B),
 C12B(H12B), C13B(H13B), C14B(H14B), C15B(H15B), C3A(H3A), C4A(H4A), C6A(H6A),
 C7A(H7A), C8A(H8A), C9A(H9A), C11A(H11A), C12A(H12A), C13A(H13A), C14A(H14A),
 C15A(H15A), C7(H7), C10(H10), C8(H8), C11(H11), C5(H5), C4(H4), C13(H13),
 C14(H14), C4C(H4C), C5C(H5C), C8C(H8C), C7C(H7C), C10C(H10C), C13C(H13C),
 C11C(H11C), C14C(H14C)
5.b Fitted hexagon refined as free rotating group:
 N2B(C3B,C4B,C5B,C6B,C7B), C10B(C11B,C12B,C13B,C14B,C15B), N2A(C3A,C4A,C5A,C6A,
 C7A), C10A(C11A,C12A,C13A,C14A,C15A)
;
_shelx_res_checksum              23412
_shelx_fab_checksum              41146
_olex2_submission_special_instructions 'No special instructions were received'