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_7043555
_publ_section_title
;
 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 Mn0.5 Mo3 N3 O13 P2), 3(C2 H3 N), C16 N'
_chemical_formula_sum            'C126 H97 Cu2 Mn Mo6 N10 O26 P4'
_chemical_formula_weight         3048.67
_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
_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                83.4393(14)
_cell_angle_beta                 78.0230(16)
_cell_angle_gamma                66.0723(18)
_cell_formula_units_Z            2
_cell_length_a                   18.4673(4)
_cell_length_b                   19.4960(3)
_cell_length_c                   25.0204(4)
_cell_measurement_reflns_used    25640
_cell_measurement_temperature    150.05(10)
_cell_measurement_theta_max      73.7260
_cell_measurement_theta_min      4.0740
_cell_volume                     8050.3(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.05(10)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            62000
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.165
_diffrn_reflns_theta_min         3.050
_exptl_absorpt_coefficient_mu    5.458
_exptl_absorpt_correction_T_max  0.203
_exptl_absorpt_correction_T_min  0.039
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Numerical absorption correction based on gaussian integration over
   a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_description       block
_exptl_crystal_F_000             3052
_exptl_crystal_preparation       MeCN
_exptl_crystal_recrystallization_method MeCN
_exptl_crystal_size_max          0.2473
_exptl_crystal_size_mid          0.1811
_exptl_crystal_size_min          0.1115
_platon_squeeze_details
;
TITL SS15097 in P-1 #2
CELL   18.4672   19.5003   25.0218     83.48     78.03     66.07
SPGR P-1
C101 0.919 0.497 0.209 !       3.27 eA-3
C102 0.409 0.344 0.443 !       3.15 eA-3
C103 0.733 0.532 0.374 !       2.82 eA-3
C104 0.833 0.142 0.049 !       2.58 eA-3
C105 0.169 0.185 0.313 !       2.56 eA-3
C106 0.462 0.159 0.170 !       2.51 eA-3
C107 0.065 0.763 0.315 !       2.43 eA-3
C108 0.731 0.454 0.141 !       2.39 eA-3
C109 0.844 0.112 0.010 !       2.39 eA-3
C110 0.985 0.766 0.324 !       2.32 eA-3
C111 0.390 0.156 0.203 !       2.31 eA-3
C112 0.950 0.269 0.353 !       2.22 eA-3
C113 0.118 0.767 0.304 !       2.09 eA-3
C114 0.902 0.077 0.012 !       2.09 eA-3
C115 0.723 0.464 0.402 !       2.08 eA-3
C116 0.948 0.434 0.170 !       2.07 eA-3
C117 0.333 0.156 0.226 !       2.05 eA-3
C118 0.820 0.175 0.276 !       1.96 eA-3
C119 0.944 0.233 0.393 !       1.94 eA-3
C120 0.500 0.644 0.469 !       1.91 eA-3
C121 0.967 0.376 0.145 !       1.87 eA-3
C122 0.383 0.407 0.444 !       1.86 eA-3
C123 0.769 0.396 0.140 !       1.71 eA-3
C124 0.444 0.361 0.491 !       1.70 eA-3
C125 0.500 0.500 0.500 !       1.67 eA-3
C126 0.964 0.029 0.009 !       1.67 eA-3
C127 0.970 0.297 0.306 !       1.62 eA-3
C128 0.735 0.216 0.403 !       1.57 eA-3
C129 0.753 0.217 0.352 !       1.57 eA-3
C130 0.565 0.422 0.313 !       1.54 eA-3
C131 0.594 0.406 0.297 !       1.52 eA-3
C132 0.623 0.387 0.293 !       1.52 eA-3
Q133 0.183 0.215 0.256 !       1.48 eA-3
C134 0.487 0.594 0.475 !       1.48 eA-3
Q135 0.262 0.406 0.236 !       1.34 eA-3
Q136 0.455 0.340 0.118 !       1.34 eA-3
Q137 0.539 0.592 0.094 !       1.25 eA-3
Q138 0.494 0.469 0.171 !       1.23 eA-3
Q139 0.194 0.375 0.251 !       1.23 eA-3
Q140 0.489 0.482 0.142 !       1.23 eA-3
Q141 0.139 0.278 0.237 !       1.20 eA-3
C142 0.724 0.406 0.412 !       1.19 eA-3
C143 0.371 0.472 0.445 !       1.19 eA-3
Q144 0.460 0.362 0.082 !       1.18 eA-3
C145 0.849 0.501 0.219 !       1.16 eA-3
Q146 0.541 0.629 0.054 !       1.14 eA-3
Q147 0.851 0.669 0.431 !       1.14 eA-3
Q148 0.149 0.345 0.447 !       1.12 eA-3
Q149 0.160 0.765 0.466 !       1.10 eA-3
C150 0.747 0.469 0.300 !       1.09 eA-3
C151 0.549 0.380 0.314 !       1.06 eA-3
Q152 0.311 0.498 0.278 !       1.06 eA-3
Q153 0.545 0.310 0.321 !       1.05 eA-3
C154 0.841 0.294 0.171 !       1.03 eA-3
Q155 0.034 0.479 0.366 !       1.02 eA-3
C156 0.775 0.483 0.237 !       1.01 eA-3
C157 0.517 0.436 0.352 !       0.96 eA-3
Q158 0.944 0.546 0.378 !       0.92 eA-3
Q159 0.498 0.488 0.038 !       0.92 eA-3
C160 0.751 0.454 0.244 !       0.92 eA-3
Q161 0.287 0.549 0.321 !       0.92 eA-3
Q162 0.540 0.643 0.015 !       0.90 eA-3
Q163 0.235 0.718 0.479 !       0.89 eA-3
Q164 0.449 0.375 0.041 !       0.89 eA-3
C165 0.744 0.470 0.213 !       0.85 eA-3
Q166 0.142 0.565 0.139 !       0.80 eA-3
Q167 0.995 0.547 0.329 !       0.80 eA-3
Q168 0.284 0.767 0.470 !       0.78 eA-3
Q169 0.235 0.094 0.005 !       0.76 eA-3
Q170 0.356 0.655 0.065 !       0.76 eA-3
Q171 0.333 0.610 0.094 !       0.75 eA-3
Q172 0.282 0.784 0.452 !       0.74 eA-3
Q173 0.494 0.512 0.100 !       0.72 eA-3
Q174 0.122 0.827 0.457 !       0.71 eA-3
Q175 0.349 0.421 0.235 !       0.71 eA-3
Q176 0.879 0.609 0.444 !       0.70 eA-3
Q177 0.990 0.486 0.369 !       0.69 eA-3
C178 0.498 0.468 0.274 !       0.69 eA-3
Q179 0.826 0.621 0.486 !       0.69 eA-3
Q180 0.922 0.327 0.057 !       0.69 eA-3
Q181 0.870 0.814 0.055 !       0.69 eA-3
Q182 0.447 0.363 0.208 !       0.68 eA-3
Q183 0.100 0.580 0.117 !       0.68 eA-3
Q184 0.152 0.421 0.378 !       0.67 eA-3
Q185 0.184 0.513 0.445 !       0.67 eA-3
Q186 0.604 0.612 0.047 !       0.67 eA-3
Q187 0.541 0.605 0.195 !       0.66 eA-3
Q188 0.406 0.236 0.152 !       0.66 eA-3
Q189 0.196 0.343 0.408 !       0.66 eA-3
Q190 0.796 0.653 0.466 !       0.65 eA-3
Q191 0.347 0.579 0.323 !       0.65 eA-3
Q192 0.246 0.837 0.441 !       0.65 eA-3
Q193 0.255 0.455 0.281 !       0.64 eA-3
Q194 0.551 0.501 0.115 !       0.64 eA-3
Q195 0.643 0.921 0.495 !       0.64 eA-3
Q196 0.193 0.638 0.470 !       0.64 eA-3
Q197 0.767 0.767 0.100 !       0.63 eA-3
Q198 0.771 0.967 0.153 !       0.63 eA-3
Q199 0.922 0.409 0.428 !       0.63 eA-3
;
_refine_diff_density_max         1.234
_refine_diff_density_min         -0.841
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1632
_refine_ls_number_reflns         31719
_refine_ls_number_restraints     478
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0583
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1006P)^2^+3.0217P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1653
_refine_ls_wR_factor_ref         0.1785
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24238
_reflns_number_total             31719
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02316b2.cif
_cod_data_source_block           ss15097_sqd
_cod_database_code               7043555
_shelxl_version_number           2014-3
_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. Restrained distances
 C115-C126
 1.45 with sigma of 0.02
 C126-C119
 1.45 with sigma of 0.02
 C121-C126
 2.55 with sigma of 0.02
 C126-C120
 2.55 with sigma of 0.02
 C122-C130
 1.5 with sigma of 0.02
 C122-C123
 2.5 with sigma of 0.02
 C130-C123
 1.5 with sigma of 0.02
3. Rigid bond restraints
 N8, C108, C109, C110, C117, C132, C124, C111, C120, C114, C118, C121, C123,
 C112, C119, C113, C116, C115, C130, C131, C126, C122, C125
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C129, C82, C83, C84, N5, C80, C81, C87, C88, C89, C91, C90, N6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N4, C128, C127, C89, C88, C87, C91, C90, N6, C80, N5, C84, C83, C82, C81, C129
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N7, C102, C106, C103, C97, N9B, C105, C107, N10B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C97, C103, N9B, C105, C107, N10B, N10A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C107, C105, N10B, N10A, C103, C97, N9B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N8 \\sim C108 \\sim C109 \\sim C110 \\sim C117 \\sim C132 \\sim C124 \\sim C111
\\sim C120 \\sim C114 \\sim C118 \\sim C121 \\sim C123 \\sim C112 \\sim C119
\\sim C113 \\sim C116 \\sim C115 \\sim C130 \\sim C131 \\sim C126 \\sim C122
\\sim C125: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
N5 \\sim C83 \\sim C84 \\sim C82 \\sim C80 \\sim C81 \\sim C87 \\sim N6 \\sim
C91 \\sim C90 \\sim C89 \\sim C88 \\sim C129: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
C128 \\sim C127 \\sim C89 \\sim C90 \\sim C88 \\sim C87 \\sim C91 \\sim N6
\\sim N5 \\sim C84 \\sim C80 \\sim C82 \\sim C81 \\sim C83 \\sim C129 \\sim N4:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
N7 \\sim C102 \\sim C106 \\sim N10B \\sim C105 \\sim C107 \\sim C97 \\sim C103
\\sim N9B: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C107 \\sim C105 \\sim N10B \\sim N10A \\sim C103 \\sim C97 \\sim N9B: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08
C103 \\sim C97 \\sim N9B \\sim C107 \\sim C105 \\sim N10B \\sim N10A: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08
5. Others
 Fixed Sof: C109(0.5) C110(0.5) N10B(0.5) C113(0.5) C114(0.5) C115(0.5)
 C119(0.5) C120(0.5) C121(0.5) C123(0.5) C124(0.5) C127(0.5) H127(0.5)
 C128(0.5) H128(0.5) C130(0.5) C132(0.5) N10A(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C2(H2a,H2b), C3(H3a,H3b), C32(H32a,H32b), C45(H45a,H45b), C53(H53a,H53b),
 C133(H13a,H13b)
6.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C11(H11), C12(H12), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19),
 C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C31(H31), C33(H33),
  C35(H35), C37(H37), C41(H41), C43(H43), C46(H46), C47(H47), C48(H48),
 C49(H49), C50(H50), C51(H51), C52(H52), C54(H54), C55(H55), C56(H56), C57(H57),
  C58(H58), C59(H59), C60(H60), C61(H61), C62(H62), C63(H63), C64(H64),
 C65(H65), C67(H67), C68(H68), C69(H69), C70(H70), C71(H71), C72(H72), C73(H73),
  C74(H74), C75(H75), C76(H76), C77(H77), C78(H78), C79(H79), C81(H81),
 C83(H83), C84(H84), C85(H85), C86(H86), C88(H88), C90(H90), C91(H91), C93(H93),
  C94(H94), C95(H95), C96(H96), C98(H98), C99(H99), C100(H100), C101(H101),
 C104(H104), C127(H127), C128(H128)
6.c Fitted hexagon refined as free rotating group:
 C80(C81,C82,C83,C84,N5), C87(C88,C89,C90,C91,N6)
6.d Idealised Me refined as rotating group:
 C66(H66a,H66b,H66c), C97(H97a,H97b,H97c), C105(H10a,H10b,H10c), C106(H10d,
 H10e,H10f), C129(H12a,H12b,H12c)
;
_shelx_res_checksum              71222
_platon_squeeze_void_probe_radius 1.20
_shelx_fab_checksum              92231
_olex2_submission_special_instructions 'No special instructions were received'