Supramolecular self-assembly for designing non-centrosymmetric crystals based on Keggin polyoxometallates and crown ether.
Xiong, Jun; Kubo, Kazuya; Lü, Shao-Fang; Li, Ming; Nakamura, Takayoshi; Dalton transactions (Cambridge, England : 2003) 47 (2018) 14001–14007; doi:10.1039/c8dt02910e

data_7701909
_publ_section_title
;
 Supramolecular self-assembly for designing non-centrosymmetric crystals
 based on Keggin polyoxometallates and crown ether.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14001
_journal_page_last               14007
_journal_paper_doi               10.1039/c8dt02910e
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety
'Mo12 O40 P, 3(C6 H7 Br N), 3(C16 H24 O6), 2(C2 H3 N)'
_chemical_formula_sum            'C70 H99 Br3 Mo12 N5 O58 P'
_chemical_formula_weight         3360.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-10-22
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-11-27 deposited with the CCDC.
2018-09-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.71(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.634(4)
_cell_length_b                   16.955(3)
_cell_length_c                   18.481(4)
_cell_measurement_reflns_used    2592
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      3
_cell_volume                     5234(2)
_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-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_unetI/netI     0.0795
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            36520
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.100
_diffrn_reflns_theta_max         25.100
_diffrn_reflns_theta_min         3.028
_exptl_absorpt_coefficient_mu    2.647
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.132
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3284
_refine_diff_density_max         2.442
_refine_diff_density_min         -1.168
_refine_diff_density_rms         0.227
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.43(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1358
_refine_ls_number_reflns         17702
_refine_ls_number_restraints     669
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0749
_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^)+(0.1202P)^2^+18.6403P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1859
_refine_ls_wR_factor_ref         0.1909
_reflns_Friedel_coverage         0.998
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                16233
_reflns_number_total             17702
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02910e2.cif
_cod_data_source_block           shelx_CCDC4
_cod_database_code               7701909
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.57(3)
 0.43(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All N(H,H,H) groups
3. Restrained distances
 C69-C70
 1.54 with sigma of 0.001
 C70-N5
 1.16 with sigma of 0.001
 C69-N5
 2.7 with sigma of 0.001
 C67-C68
 1.54 with sigma of 0.001
 C68-N4
 1.16 with sigma of 0.001
 C67-N4
 2.7 with sigma of 0.001
 C9-C10
 1.5 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C69) \\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(C67)
\\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(N4) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(O56) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C11)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Br2A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C67, C68, N4, C69, C70, N5
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C13, C14, C15, C16, C17,
 C18, C19, C20, C21, C22, C23, C24, C25, C26, C27, C28, C29, C30, C31, C32, C33,
  C34, C35, C36, C37, C38, C39, C40, C41, C42, C43, C44, C45, C46, C47, C48,
 C49, C50, C51, C52, C53, C54, C55, C56, C57, C58, C59, C60, C61, C62, C63, C64,
  C65, C66, C67, C68, C69, C70, N1, N2, N3, N4, N5, O1, O2, O3, O4, O5, O6, O7,
 O8, O9, O10, O11, O12, O13, O14, O15, O16, O17, O18, O19, O20, O21, O22, O23,
 O24, O25, O26, O27, O28, O29, O30, O31, O32, O33, O34, O35, O36, O37, O38, O39,
  O40, O41, O42, O43, O44, O45, O46, O47, O48, O49, O50, O51, O52, O53, O54,
 O55, O56, O57, O58
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(Br2A)=1-FVAR(1)
 Sof(Br2)=FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B),
  C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,
 H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B),
 C38(H38A,H38B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B),
  C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B), C59(H59A,
 H59B), C60(H60A,H60B)
7.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C18(H18), C19(H19), C21(H21), C22(H22),
 C24(H24), C25(H25), C26(H26), C27(H27), C40(H40), C41(H41), C43(H43), C44(H44),
  C46(H46), C47(H47), C48(H48), C49(H49), C62(H62), C63(H63), C65(H65), C66(H66)
7.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(H2A,H2B,H2C), N3(H3A,H3B,H3C), C67(H67A,H67B,H67C),
 C69(H69A,H69B,H69C)
;
_olex2_submission_special_instructions 'No special instructions were received'