Influence of interpenetration on the flexibility of MUV-2
Vicent-Morales, María; Vitórica-Yrezábal, Iñigo J.; Souto, Manuel; Mínguez Espallargas, Guillermo; CrystEngComm 21 (2019) 3031–; doi:10.1039/C9CE00233B

data_7234941
_publ_section_title
;
 Influence of interpenetration on the flexibility of MUV-2
;
_journal_issue                   19
_journal_name_full               CrystEngComm
_journal_page_first              3031
_journal_paper_doi               10.1039/C9CE00233B
_journal_volume                  21
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C66 H39 Fe3 N3 O13 S6, 1.36(C5 H5 N)'
_chemical_formula_sum            'C72.79 H45.79 Fe3 N4.36 O13 S6'
_chemical_formula_weight         1549.35
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-11-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-15 deposited with the CCDC.	2019-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.2069(7)
_cell_length_b                   57.0341(9)
_cell_length_c                   12.1673(2)
_cell_measurement_reflns_used    21972
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.5080
_cell_measurement_theta_min      1.6200
_cell_volume                     23737.9(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14d (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14d (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14d (Rigaku OD, 2018)'
_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      100
_diffrn_detector                 'Pilatus 3M detector'
_diffrn_detector_area_resol_mean 0.0350
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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   -145.00  24.00   1.00    0.20    --   30.00   0.00   0.00  169
  2  \w   -145.00  24.00   1.00    0.20    --   30.00   0.00 120.00  169
  3  \w   -145.00  24.00   1.00    0.20    --   30.00   0.00 240.00  169
  4  \f      0.00 179.00   1.00    0.20   0.00   0.00   0.00    --   179
;
_diffrn_measurement_device       'CrystalLogic Kappa (4 circle)'
_diffrn_measurement_device_type
'dectris-CrysAlisPro-abstract goniometer imported dectris images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0049900000
_diffrn_orient_matrix_UB_12      -0.0090775000
_diffrn_orient_matrix_UB_13      -0.0346097000
_diffrn_orient_matrix_UB_21      0.0157651000
_diffrn_orient_matrix_UB_22      0.0026045000
_diffrn_orient_matrix_UB_23      -0.0330454000
_diffrn_orient_matrix_UB_31      0.0115017000
_diffrn_orient_matrix_UB_32      -0.0075318000
_diffrn_orient_matrix_UB_33      0.0302393000
_diffrn_radiation_collimation    '0.3 x 1.5 Double Pinhole'
_diffrn_radiation_monochromator  Synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.1330
_diffrn_reflns_av_unetI/netI     0.0744
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       68
_diffrn_reflns_limit_k_min       -68
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            141606
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         24.519
_diffrn_reflns_theta_min         1.756
_diffrn_source                   Synchrotron
_diffrn_source_type              'Undulator, I19, DLS, RAL'
_exptl_absorpt_coefficient_mu    0.461
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63964
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14d (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.867
_exptl_crystal_description       block
_exptl_crystal_F_000             6328
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.629
_refine_diff_density_min         -1.182
_refine_diff_density_rms         0.135
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.49(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.370
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1114
_refine_ls_number_reflns         21742
_refine_ls_number_restraints     2130
_refine_ls_restrained_S_all      1.354
_refine_ls_R_factor_all          0.1221
_refine_ls_R_factor_gt           0.1143
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3166
_refine_ls_wR_factor_ref         0.3262
_reflns_Friedel_coverage         0.854
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                19109
_reflns_number_total             21742
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00233b2.cif
_cod_data_source_block           m_muv_2_py_col1_orthoc
_cod_database_code               7234941
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'FeN4C30H20O S'
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.982
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.51(4)
 0.49(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 C41-C1
 1.5 with sigma of 0.002
 S1-C8 \\sim S1A-C8
 with sigma of 0.02
 S1-C7 \\sim S1A-C7
 with sigma of 0.02
 S4-C17 \\sim S4A-C17
 with sigma of 0.02
 S4-C19 \\sim S4A-C19
 with sigma of 0.02
 S5-C54 \\sim S5A-C54
 with sigma of 0.02
 S5-C52 \\sim S5A-C52
 with sigma of 0.02
 S6-C53 \\sim S6A-C53
 with sigma of 0.02
 S6-C52 \\sim S6A-C52
 with sigma of 0.02
 C9-C10 \\sim C9-C10A
 with sigma of 0.002
 C3A-C2 \\sim C3-C2
 with sigma of 0.002
 C7-C6A \\sim C7-C6
 with sigma of 0.002
 Fe2-N2A \\sim Fe2-N2
 with sigma of 0.002
 C14A-C13 \\sim C14-C13A
 with sigma of 0.002
4. Restrained planarity
 C13A, C14, O6, O7
 with sigma of 0.002
5. Uiso/Uaniso restraints and constraints
C67 \\sim C66 \\sim C1AA \\sim N65 \\sim C4 \\sim C64: within 2A with sigma of
0.002 and sigma for terminal atoms of 0.004
C67: within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004
S4A \\sim S4 \\sim S1A \\sim S1: within 2A with sigma of 0.002 and sigma for
terminal atoms of 0.004
S6 \\sim S6A \\sim S5 \\sim S5A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
N1 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C36 \\sim N1A \\sim C37A \\sim
C38A \\sim C39A \\sim C40A \\sim C36A: within 2A with sigma of 0.002 and sigma
for terminal atoms of 0.004
C69 \\sim C46 \\sim C68 \\sim C45 \\sim C44 \\sim N2: within 2A with sigma of
0.002 and sigma for terminal atoms of 0.004
C46 \\sim C68 \\sim C45 \\sim C69 \\sim C44 \\sim C44A \\sim C69A \\sim C45A
\\sim C68A \\sim C46A \\sim N2 \\sim N2A: within 2A with sigma of 0.002 and
sigma for terminal atoms of 0.004
C56 \\sim C55 \\sim C61 \\sim C60 \\sim C58 \\sim C57: within 2A with sigma of
0.002 and sigma for terminal atoms of 0.004
N1BA \\sim C0AA \\sim C9AA \\sim C8AA \\sim C7AA \\sim C2BA: within 2A with
sigma of 0.002 and sigma for terminal atoms of 0.004
C13 \\sim C15 \\sim C16 \\sim C10 \\sim C11 \\sim C12 \\sim C15A \\sim C13A
\\sim C12A \\sim C11A \\sim C10A \\sim C16A: within 2A with sigma of 0.002 and
sigma for terminal atoms of 0.004
C28 \\sim C33A \\sim C33 \\sim C32 \\sim C32A \\sim C29 \\sim C29A \\sim C28A:
within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004
C22 \\sim C25A \\sim C26A \\sim C26 \\sim C25 \\sim C22A \\sim C21A: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08
C22 \\sim C21 \\sim C20 \\sim C20A \\sim C26 \\sim C21A \\sim C22A \\sim C23A
\\sim C23 \\sim C25 \\sim C25A \\sim C26A: within 2A with sigma of 0.002 and
sigma for terminal atoms of 0.004
C49 \\sim C48 \\sim C47 \\sim N3 \\sim C51 \\sim C50: within 2A with sigma of
0.002 and sigma for terminal atoms of 0.004
C51 \\sim N3 \\sim C47 \\sim C48 \\sim C49 \\sim C50 \\sim C51A \\sim C50A
\\sim C49A \\sim C48A \\sim C47A \\sim N3A: within 2A with sigma of 0.002 and
sigma for terminal atoms of 0.004
C14 \\sim C14A: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
O6 \\sim C14 \\sim C14A \\sim O7: within 2A with sigma of 0.002 and sigma for
terminal atoms of 0.004
Uanis(C3A) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
6. Rigid body (RIGU) restrains
 S5, S6, C52, S5A, C53, C54, S6A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 N1, C37, C38, C39, C40, C36, N1A, C37A, C38A, C39A, C40A, C36A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C49, C48, C47, N3, C51, C50
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C63, Fe3, O1, O4, O3, N1, Fe1, Fe2, C2, C1, C37, C36, O5, N3, O2, N2, C3, C3A,
  C41, C38, C40, C47, C51, C46, C44, C35, C5CA, C4A, C35A, C42, C43, C39, C48,
 C50, C68, C69, C34, C5, C5A, C34A, C2AA, C49, C45, C6, C6A, C62, C7, C53, S1,
 C9, S6, C54, C8, S2, C10, C10A, C52, S5, C55, C17, C16, C11, C11A, C16A, C61,
 C56, S3, S4, C15, C12, C12A, C15A, C60, C57, C18, C19, C27, C13, C13A, C58,
 C27A, C20, C33, C28, C14, C59, C33A, C28A, C26A, C21A, C26, C21, C32, C29, O6,
 O7, O12, O13, C32A, C29A, C25A, C22A, C25, C22, C30, C30A, C23, C31, C24, O11,
 O10, O8, O9
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C14, H28A, C14A, O6, Fe1, Fe3, O1, Fe2
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
7. Others
 Sof(C29A)=Sof(H29A)=Sof(C30A)=Sof(C32A)=Sof(H32A)=Sof(C33A)=Sof(H33A)=
 Sof(C27A)=Sof(C28A)=Sof(H28A)=1-FVAR(1)
 Sof(C29)=Sof(H29)=Sof(C30)=Sof(C32)=Sof(H32)=Sof(C33)=Sof(H33)=Sof(C27)=
 Sof(C28)=Sof(H28)=FVAR(1)
 Sof(C20A)=Sof(C21A)=Sof(H21A)=Sof(C22A)=Sof(H22A)=Sof(C23A)=Sof(C25A)=
 Sof(H25A)=Sof(C26A)=Sof(H26A)=1-FVAR(2)
 Sof(C23)=Sof(C25)=Sof(H25)=Sof(C26)=Sof(H26)=Sof(C20)=Sof(C21)=Sof(H21)=
 Sof(C22)=Sof(H22)=FVAR(2)
 Sof(C15A)=Sof(H15A)=Sof(C13A)=Sof(C12A)=Sof(H12A)=Sof(C11A)=Sof(H11A)=
 Sof(C10A)=Sof(C16A)=Sof(H16A)=Sof(C2BA)=Sof(H2BA)=Sof(N1BA)=Sof(C0AA)=
 Sof(H0AA)=Sof(C9AA)=Sof(H9AA)=Sof(C8AA)=Sof(H8AA)=Sof(C7AA)=Sof(H7AA)=
 Sof(C14A)=Sof(C51A)=Sof(H51A)=Sof(C50A)=Sof(H50A)=Sof(C49A)=Sof(H49A)=
 Sof(C48A)=Sof(H48A)=Sof(C47A)=Sof(H47A)=Sof(N3A)=1-FVAR(3)
 Sof(C14)=Sof(C13)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16)=Sof(C10)=Sof(C11)=
 Sof(H11)=Sof(C12)=Sof(H12)=Sof(C51)=Sof(H51)=Sof(N3)=Sof(C47)=Sof(H47)=
 Sof(C48)=Sof(H48)=Sof(C49)=Sof(H49)=Sof(C50)=Sof(H50)=FVAR(3)
 Sof(C3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(C34A)=Sof(H34A)=
 Sof(C35A)=Sof(H35A)=1-FVAR(4)
 Sof(C6)=Sof(C34)=Sof(H34)=Sof(C35)=Sof(H35)=Sof(C3)=Sof(C5CA)=Sof(H5CA)=
 Sof(C5)=Sof(H5)=FVAR(4)
 Sof(N1A)=Sof(C37A)=Sof(H37A)=Sof(C38A)=Sof(H38A)=Sof(C39A)=Sof(H39A)=
 Sof(C40A)=Sof(H40A)=Sof(C36A)=Sof(H36A)=1-FVAR(5)
 Sof(N1)=Sof(C37)=Sof(H37)=Sof(C38)=Sof(H38)=Sof(C39)=Sof(H39)=Sof(C40)=
 Sof(H40)=Sof(C36)=Sof(H36)=FVAR(5)
 Sof(S4A)=Sof(S1A)=1-FVAR(6)
 Sof(S1)=Sof(S4)=FVAR(6)
 Sof(S6)=Sof(S5A)=1-FVAR(7)
 Sof(S5)=Sof(S6A)=FVAR(7)
 Sof(N2A)=Sof(C46A)=Sof(H46A)=Sof(C68A)=Sof(H68A)=Sof(C45A)=Sof(H45A)=
 Sof(C69A)=Sof(H69A)=Sof(C44A)=Sof(H44A)=1-FVAR(8)
 Sof(C46)=Sof(H46)=Sof(C68)=Sof(H68)=Sof(C45)=Sof(H45)=Sof(C69)=Sof(H69)=
 Sof(C44)=Sof(H44)=Sof(N2)=FVAR(8)
8.a Aromatic/amide H refined with riding coordinates:
 C37(H37), C38(H38), C39(H39), C40(H40), C36(H36), C25(H25), C26(H26),
 C21(H21), C22(H22), C60(H60), C61(H61), C56(H56), C57(H57), C63(H63), C42(H42),
  C43(H43), C2AA(H2AA), C34(H34), C35(H35), C5CA(H5CA), C5(H5), C29(H29),
 C32(H32), C33(H33), C28(H28), C15(H15), C16(H16), C11(H11), C12(H12), C51(H51),
  C47(H47), C48(H48), C49(H49), C50(H50), C46(H46), C68(H68), C45(H45),
 C69(H69), C44(H44), C29A(H29A), C32A(H32A), C33A(H33A), C28A(H28A), C15A(H15A),
  C12A(H12A), C11A(H11A), C16A(H16A), C4A(H4A), C5A(H5A), C34A(H34A),
 C35A(H35A), C1AA(H1AA), C66(H66), C67(H67), C64(H64), C4(H4), C2BA(H2BA),
 C0AA(H0AA), C9AA(H9AA), C8AA(H8AA), C7AA(H7AA), C37A(H37A), C38A(H38A),
 C39A(H39A), C40A(H40A), C36A(H36A), C21A(H21A), C22A(H22A), C25A(H25A),
 C26A(H26A), C46A(H46A), C68A(H68A), C45A(H45A), C69A(H69A), C44A(H44A),
 C51A(H51A), C50A(H50A), C49A(H49A), C48A(H48A), C47A(H47A)
8.b Fitted hexagon refined as free rotating group:
 N1(C37,C38,C39,C40,C36), C23(C25,C26,C20,C21,C22), C58(C60,C61,C55,C56,C57),
 C62(C63,C42,C41,C43,C2AA), C6(C34,C35,C3,C5CA,C5), C29(C30,C32,C33,C27,C28),
 C13(C15,C16,C10,C11,C12), C51(N3,C47,C48,C49,C50), C46(C68,C45,C69,C44,N2),
 C29A(C30A,C32A,C33A,C27A,C28A), C15A(C13A,C12A,C11A,C10A,C16A), C3A(C4A,C5A,
 C6A,C34A,C35A), C1AA(C66,C67,C64,C4,N65), C2BA(N1BA,C0AA,C9AA,C8AA,C7AA),
 N1A(C37A,C38A,C39A,C40A,C36A), C20A(C21A,C22A,C23A,C25A,C26A), N2A(C46A,C68A,
 C45A,C69A,C44A), C51A(C50A,C49A,C48A,C47A,N3A)
;
_shelx_res_checksum              94060
_shelx_fab_checksum              34521
_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 1.329
_oxdiff_exptl_absorpt_empirical_full_min 0.586