Structural and reactivity insights into covalently linked Cu(I) complex-Anderson polyoxometalates
Schönweiz, Stefanie; Sorsche, Dieter; Schwarz, Benjamin; Rau, Sven; Streb, Carsten; Dalton Trans.  (2017) –; doi:10.1039/C7DT02316B

data_7043556
_publ_section_title
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 Structural and reactivity insights into covalently linked Cu(I)
 complex-Anderson polyoxometalates
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02316B
_journal_year                    2017
_chemical_formula_moiety
'2(C52 H44 Cu Fe0.5 Mo3 N3 O13 P2), C16 H36 N, C3 H7 N O'
_chemical_formula_sum            'C123 H131 Cu2 Fe Mo6 N8 O27 P4'
_chemical_formula_weight         3035.80
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2017-06-12
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-06-25 deposited with the CCDC.
2017-07-07 downloaded from the CCDC.
;
_cell_angle_alpha                76.188(2)
_cell_angle_beta                 84.685(2)
_cell_angle_gamma                77.648(3)
_cell_formula_units_Z            2
_cell_length_a                   17.4451(10)
_cell_length_b                   20.8647(12)
_cell_length_c                   23.6902(12)
_cell_measurement_reflns_used    9571
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      2.34
_cell_volume                     8171.9(8)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      149.99
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0824
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            240959
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.401
_diffrn_reflns_theta_min         2.043
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.882
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6893
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0763 before and 0.0665 after correction. The Ratio of minimum to maximum transmission is 0.9247. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       thin
_exptl_crystal_F_000             3074
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.372
_refine_diff_density_min         -1.008
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1512
_refine_ls_number_reflns         33407
_refine_ls_number_restraints     258
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.1026
_refine_ls_R_factor_gt           0.0779
_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^)+(0.0437P)^2^+96.8780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1784
_refine_ls_wR_factor_ref         0.1954
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25069
_reflns_number_total             33407
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02316b2.cif
_cod_data_source_block           bs17027_0m
_cod_database_code               7043556
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. 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
2. Rigid bond restraints
 N8, C112, C113, C114, O26, N8, C112, N8, C113, N8, C114, O26, C114, N7, C57,
 C58, C63, C67, C60, C76, C95, C75, C72, C74, C111, C97, C79, C116, C115, C102,
 N7, C57, N7, C58, N7, C63, N7, C67, C60, C57, C76, C58, C95, C63, C75, C67,
 C72, C60, C74, C76, C95, C111, C97, C75, C72, C79, C74, C116, C115, C111, C102,
  C97
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C117, C122, C121, C120, C119, C118
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C99, C83, C59, C62, C100, C109
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
N7 \\sim C57 \\sim C58 \\sim C63 \\sim C67 \\sim C60 \\sim C76 \\sim C95 \\sim
C75 \\sim C72 \\sim C74 \\sim C111 \\sim C97 \\sim C79 \\sim C116 \\sim C115
\\sim C102 \\sim N7 \\sim C57 \\sim N7 \\sim C58 \\sim N7 \\sim C63 \\sim N7
\\sim C67 \\sim C60 \\sim C57 \\sim C76 \\sim C58 \\sim C95 \\sim C63 \\sim C75
\\sim C67 \\sim C72 \\sim C60 \\sim C74 \\sim C76 \\sim C95 \\sim C111 \\sim
C97 \\sim C75 \\sim C72 \\sim C79 \\sim C74 \\sim C116 \\sim C115 \\sim C111
\\sim C102 \\sim C97 \\sim N8 \\sim C112 \\sim C113 \\sim C114 \\sim O26 \\sim
N8 \\sim C112 \\sim N8 \\sim C113 \\sim N8 \\sim C114 \\sim O26 \\sim C114:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C117 \\sim C118 \\sim C119 \\sim C120 \\sim C121 \\sim C122: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C83 \\sim C59 \\sim C62 \\sim C100 \\sim C109 \\sim C99: within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08
4.a Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C2(H2a,H2b), C3(H3a,H3b), C6(H6a,H6b), C9(H9a,H9b), C57(H57a,
 H57b), C58(H58a,H58b), C60(H60a,H60b), C63(H63a,H63b), C67(H67a,H67b),
 C72(H72a,H72b), C74(H74a,H74b), C75(H75a,H75b), C76(H76a,H76b), C95(H95a,H95b),
  C97(H97a,H97b), C111(H11a,H11b), C123(H12a,H12b)
4.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C14(H14), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20),
 C25(H25), C26(H26), C27(H27), C28(H28), C31(H31), C32(H32), C33(H33), C34(H34),
  C35(H35), C36(H36), C37(H37), C39(H39), C40(H40), C41(H41), C46(H46),
 C47(H47), C49(H49), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55), C64(H64),
  C65(H65), C66(H66), C68(H68), C69(H69), C70(H70), C71(H71), C73(H73),
 C78(H78), C80(H80), C81(H81), C82(H82), C84(H84), C85(H85), C86(H86), C87(H87),
  C88(H88), C89(H89), C90(H90), C91(H91), C92(H92), C93(H93), C94(H94),
 C99(H99), C83(H83), C62(H62), C100(H100), C109(H109), C101(H101), C103(H103),
 C104(H104), C105(H105), C107(H107), C108(H108), C110(H110), C114(H114),
 C117(H117), C119(H119), C120(H120), C121(H121), C122(H122)
4.c Fitted hexagon refined as free rotating group:
 C99(C83,C59,C62,C100,C109), C117(C118,C119,C120,C121,C122)
4.d Idealised Me refined as rotating group:
 C38(H38a,H38b,H38c), C79(H79a,H79b,H79c), C102(H10d,H10e,H10f), C106(H10a,
 H10b,H10c), C112(H11i,H11j,H11k), C113(H11l,H11m,H11n), C115(H11c,H11d,H11e),
 C116(H11f,H11g,H11h)
;
_shelx_res_checksum              28540
_shelx_fab_checksum              85409
_olex2_submission_special_instructions 'No special instructions were received'