Self-Assembly and Ionic-Lattice-like Secondary Structure of a Flexible Linear Polymer of Highly Charged Inorganic Building Blocks.
Zhang, Guanyun; Gadot, Eyal; Gan-Or, Gal; Baranov, Mark; Tubul, Tal; Neyman, Alevtina; Li, Mu; Clotet, Anna; Poblet, Josep M.; Yin, Panchao; Weinstock, Ira A.; Journal of the American Chemical Society 142 (2020) 7295–7300; doi:10.1021/jacs.0c01486

data_4134674
_publ_section_title
;
 Self-Assembly and Ionic-Lattice-like Secondary Structure of a Flexible
 Linear Polymer of Highly Charged Inorganic Building Blocks.
;
_journal_issue                   16
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7295
_journal_page_last               7300
_journal_paper_doi               10.1021/jacs.0c01486
_journal_volume                  142
_journal_year                    2020
_chemical_formula_moiety
'Mo10 Nb2 O40 P, 2(C24 H52 N), C24 H42 N, C23 H45 N, 2(C4 H8 O)'
_chemical_formula_sum            'C103 H207 Mo10 N4 Nb2 O42 P'
_chemical_formula_weight         3349.90
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-05
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_cell_angle_alpha                90
_cell_angle_beta                 103.1750(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.4887(2)
_cell_length_b                   22.9828(2)
_cell_length_c                   21.1268(2)
_cell_measurement_reflns_used    87225
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      32.9710
_cell_measurement_theta_min      2.6010
_cell_volume                     6849.86(13)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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    -84.00   7.00   0.50   15.00    --  -11.46 -66.00 112.00  182
  2  \w    -26.00  22.00   0.50   15.00    --  -11.46 -99.00 150.00   96
  3  \w     36.00  82.00   0.50   15.00    --    9.90-178.00  90.00   92
  4  \w    -26.00  22.00   0.50   15.00    --  -11.46 -99.00 -30.00   96
  5  \w    -26.00  43.00   0.50   15.00    --    9.90 -99.00  90.00  138
  6  \w     -2.00  83.00   0.50   15.00    --    9.90  38.00 -90.00  170
  7  \w    -30.00  61.00   0.50   15.00    --  -11.46  66.00-113.00  182
  8  \w    -34.00  61.00   0.50   15.00    --  -11.46  77.00 -60.00  190
  9  \w    -26.00  33.00   0.50   15.00    --  -11.46  57.00  90.00  118
 10  \w    -26.00  61.00   0.50   15.00    --  -11.46  57.00 150.00  174
 11  \w    -84.00   4.00   0.50   15.00    --  -11.46 -57.00 -60.00  176
 12  \w     36.00  82.00   0.50   15.00    --    9.90-178.00-180.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            152719
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.059
_diffrn_reflns_theta_max         25.059
_diffrn_reflns_theta_min         2.286
_exptl_absorpt_coefficient_mu    1.128
_exptl_absorpt_correction_T_max  0.176
_exptl_absorpt_correction_T_min  0.089
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_description       prism
_exptl_crystal_F_000             3412
_exptl_crystal_size_max          0.221
_exptl_crystal_size_mid          0.183
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.598
_refine_diff_density_min         -1.417
_refine_diff_density_rms         0.133
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.49(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     936
_refine_ls_number_reflns         24202
_refine_ls_number_restraints     156
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0621
_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^)+(0.0610P)^2^+52.7463P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1503
_refine_ls_wR_factor_ref         0.1541
_reflns_Friedel_coverage         0.948
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                22364
_reflns_number_total             24202
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c01486_si_001.cif
_cod_data_source_block           pnb2mo10o40_mo_100k
_cod_depositor_comments          'Adding full bibliography for 4134674.cif.'
_cod_database_code               4134674
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.831
_shelx_estimated_absorpt_t_min   0.789
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.51(8)
 0.49(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Shared sites
{Mo11, Nb3}
{Mo10, Nb2}
4. Restrained distances
 C74-C73 = C74-C44 = C63-C44
 1.54 with sigma of 0.01
 C67-C92 = C85-C67 = C85-C82 = C82-C60
 1.54 with sigma of 0.01
 C95-C51 = C95-C26
 1.54 with sigma of 0.01
 C57-C56
 1.54 with sigma of 0.01
 C54-C49 = C49-C7
 1.54 with sigma of 0.01
 C87-C54
 1.54 with sigma of 0.01
 C70-C59 = C59-C58
 1.54 with sigma of 0.01
 C5-C48 = C61-C48 = C61-C46 = C9-C46 = C9-C52 = C14-C10 = C21-C10 = C21-C15 =
 C41-C15 = C68-C41 = C6-C37 = C76-C37 = C76-C50 = C53-C50 = C53-C31 = C4-C13 =
 C8-C13 = C8-C56 = C57-C56 = C79-C57
 1.54 with sigma of 0.01
 C39-C32 = C62-C32 = C82-C60 = C85-C82 = C85-C67 = C92-C67 = C88-C80 = C88-C99
 = C83-C99 = C86-C83 = C86-C77 = C58-C23 = C59-C58 = C70-C59 = C70-C69 = C93-C69
 1.54 with sigma of 0.01
 C28-C12 = C7-C12 = C7-C49 = C54-C49 = C87-C54 = C36-C3 = C3-C1 = C2-C1 = C29-
 C2 = C29-C11 = C34-C16 = C34-C17 = C22-C17 = C25-C22 = C45-C25 = C38-C19 = C64-
 C19 = C64-C35 = C42-C35 = C42-C33
 1.54 with sigma of 0.01
 C27-C20 = C63-C27 = C63-C44 = C74-C44 = C74-C73 = C94-C72 = C94-C43 = C43-C98
 = C81-C98 = C55-C26 = C95-C26 = C95-C51 = C65-C51 = C75-C65 = C47-C30 = C97-
 C30 = C97-C71 = C96-C71 = C47-C18
 1.54 with sigma of 0.01
 C89-C84 = C89-C66 = C66-C40
 1.54 with sigma of 0.01
 C92-C100
 1.54 with sigma of 0.01
 C90-C78 = C91-C90 = C78-C24
 1.54 with sigma of 0.01
 O41-C24 = O41-C91
 1.43 with sigma of 0.01
 C102-C99 = C103-C102 = C77-C103
 1.54 with sigma of 0.01
 C105-C104 = C106-C105 = C106-C62
 1.54 with sigma of 0.01
 Mo2-O3
 2.46 with sigma of 0.001
 Nb1-O32 = Nb1-O22 = Nb1-O14 = Nb1-O24
 2.05 with sigma of 0.005
 Nb1-O23
 1.67 with sigma of 0.001
 Nb2-O22 = Nb2-O33 = Nb2-O20 = Nb2-O15
 1.99 with sigma of 0.003
 Nb2-O21
 1.66 with sigma of 0.001
 Nb3-O39 = Nb3-O33 = Nb3-O35 = Nb3-O34
 1.98 with sigma of 0.003
 Nb3-O38
 1.65 with sigma of 0.001
 C82-C67
 2.5 with sigma of 0.04
 C67-C82
 2.5 with sigma of 0.04
 C82-C86
 4 with sigma of 0.04
 C102-C88
 2.5 with sigma of 0.04
5. Uiso/Uaniso restraints and constraints
Uanis(C23) = Uanis(C58) = Uanis(C59) = Uanis(C70) = Uanis(C69) = Uanis(C93)
Uanis(C18) = Uanis(C47) = Uanis(C30) = Uanis(C97) = Uanis(C71) = Uanis(C96)
Uanis(C43) = Uanis(C98) = Uanis(C81) = Uanis(C94) = Uanis(C72)
Uanis(C54) = Uanis(C87) = Uanis(C49) = Uanis(C7) = Uanis(C12) = Uanis(C28)
Uanis(C60) = Uanis(C82) = Uanis(C64) = Uanis(C67) = Uanis(C92) = Uanis(C100) =
Uanis(C101)
Uanis(C80) = Uanis(C88) = Uanis(C99) = Uanis(C83) = Uanis(C86) = Uanis(C77) =
Uanis(N2) = Uanis(C62) = Uanis(C32) = Uanis(C39) = Uanis(C104) = Uanis(C102) =
Uanis(C103) = Uanis(C105) = Uanis(C106)
Uanis(C31) = Uanis(C53) = Uanis(C50) = Uanis(C76) = Uanis(C37) = Uanis(C6)
Uanis(C75) = Uanis(C65) = Uanis(C51) = Uanis(C95) = Uanis(C26) = Uanis(C55)
Uanis(C4) = Uanis(C13) = Uanis(C8) = Uanis(C56) = Uanis(C57) = Uanis(C79)
Uanis(C45) = Uanis(C25) = Uanis(C22) = Uanis(C17) = Uanis(C34) = Uanis(C16) =
Uanis(C38) = Uanis(N1)
Uanis(O12) = Uanis(O28) = Uanis(O26) = Uanis(O30) = Uanis(O40) = Uanis(O29) =
Uanis(O35) = Uanis(O34) = Uanis(O22) = Uanis(O20) = Uanis(O14) = Uanis(O8) =
Uanis(O13) = Uanis(O6) = Uanis(O15)
Uanis(C33) = Uanis(C42) = Uanis(C35) = Uanis(C64) = Uanis(C19) = Uanis(C38)
Uanis(C73) = Uanis(C74) = Uanis(C44) = Uanis(C63) = Uanis(C27) = Uanis(C20)
Uanis(Mo11) = Uanis(Nb3)
Uanis(Mo10) = Uanis(Nb2)
Uanis(O41) = Uanis(C91) = Uanis(C90) = Uanis(C78) = Uanis(C24) = Uanis(C40) =
Uanis(O42) = Uanis(C84) = Uanis(C89) = Uanis(C66)
6. Rigid body (RIGU) restrains
 C96, C47, C95, C91, C90, C47, C67, C85, C92, C100, C33, C42, C35, C89, C84
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
7. Others
 Fixed Sof: Mo11(0.7) Mo10(0.3) H62A(0.5) H62B(0.5) C67(0.5) C83(0.5)
 H83A(0.5) H83B(0.5) H85C(0.5) H85D(0.5) H85A(0.5) H85B(0.5) C86(0.5) H86A(0.5)
 H86B(0.5) H92A(0.5) H92B(0.5) H99A(0.5) H99B(0.5) H99C(0.5) H99D(0.5)
 C101(0.5) H10D(0.5) H10E(0.5) C102(0.5) C103(0.5) H10F(0.5) H10G(0.5) Nb3(0.3)
 Nb2(0.7)
8.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10L,H10M), C12(H12A,H12B),
 C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B),
  C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,
 H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B),
 C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C32(H32A,H32B), C34(H34A,H34B),
  C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,
 H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B),
 C44(H44A,H44B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B),
  C50(H50A,H50B), C51(H51A,H51B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,
 H55B), C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B),
 C60(H60A,H60B), C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B), C64(H64A,H64B),
  C65(H65A,H65B), C66(H66A,H66B), C69(H69A,H69B), C70(H70A,H70B), C71(H71A,
 H71B), C72(H72A,H72B), C74(H74A,H74B), C76(H76A,H76B), C78(H78A,H78B),
 C80(H80A,H80B), C82(H82A,H82B), C83(H83A,H83B), C84(H84A,H84B), C85(H85C,H85D),
  C85(H85A,H85B), C86(H86A,H86B), C88(H88A,H88B), C89(H89A,H89B), C90(H90A,
 H90B), C91(H91A,H91B), C92(H92A,H92B), C94(H94A,H94B), C95(H95A,H95B),
 C97(H97A,H97B), C98(H98A,H98B), C99(H99A,H99B), C99(H99C,H99D), C101(H10D,
 H10E), C103(H10F,H10G), C105(H10H,H10I), C106(H10J,H10K)
8.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C45(H45A,H45B,
 H45C), C52(H52A,H52B,H52C), C68(H68A,H68B,H68C), C75(H75A,H75B,H75C), C79(H79A,
 H79B,H79C), C81(H81A,H81B,H81C), C87(H87A,H87B,H87C), C93(H93A,H93B,H93C),
 C96(H96A,H96B,H96C), C100(H10A,H10B,H10C)
;
_olex2_submission_special_instructions 'No special instructions were received'