Assembly, disassembly and reassembly: a "top-down" synthetic strategy towards hybrid, mixed-metal {Mo<sub>10</sub>Co<sub>6</sub>} POM clusters.
Healy, Colm; Steuber, Friedrich W.; Wix, Paul; Macreadie, Lauren K.; Kathalikkattil, Amal Cherian; Schmitt, Wolfgang; Dalton transactions (Cambridge, England : 2003) 48 (2019) 3018–3027; doi:10.1039/c9dt00075e

data_7048878
_publ_section_title
;
 Assembly, disassembly and reassembly: a &quot;top-down&quot; synthetic
 strategy towards hybrid, mixed-metal {Mo<sub>10</sub>Co<sub>6</sub>} POM
 clusters.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3018
_journal_page_last               3027
_journal_paper_doi               10.1039/c9dt00075e
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety
'C48 H68 Co3 Mo5 N2 O29 P3, C43 H63 Co3 Mo5 N O29 P3, 2(C16 H36 N), 5(C2 N)'
_chemical_formula_sum            'C133 H203 Co6 Mo10 N10 O58 P6'
_chemical_formula_weight         4368.84
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-10-09
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-11-02 deposited with the CCDC.
2019-02-05 downloaded from the CCDC.
;
_cell_angle_alpha                75.8350(10)
_cell_angle_beta                 80.8820(10)
_cell_angle_gamma                72.5210(10)
_cell_formula_units_Z            2
_cell_length_a                   17.7506(7)
_cell_length_b                   18.8983(8)
_cell_length_c                   27.1892(12)
_cell_measurement_reflns_used    9833
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.45
_cell_measurement_theta_min      2.31
_cell_volume                     8399.5(6)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0895
_diffrn_reflns_av_unetI/netI     0.0692
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            202902
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.497
_diffrn_reflns_theta_min         1.374
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.435
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6806
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0604 before and 0.0548 after correction. The Ratio of minimum to maximum transmission is 0.9131. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.727
_exptl_crystal_description       block
_exptl_crystal_F_000             4414
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.937
_refine_diff_density_min         -1.831
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1956
_refine_ls_number_reflns         34616
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0883
_refine_ls_R_factor_gt           0.0439
_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^)+(0.0480P)^2^+23.6040P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.1160
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23350
_reflns_number_total             34616
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00075e2.cif
_cod_data_source_block           fs025
_cod_depositor_comments
'Adding full bibliography for 7048870--7048879.cif.'
_cod_database_code               7048878
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.906
_shelx_estimated_absorpt_t_min   0.824
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H01G(0.034) H01H(0.034) H01A(0.032) H01B(0.032) H01I(0.033)
 H01J(0.033) H01C(0.034) H01D(0.034) H01E(0.038) H01F(0.038) H01K(0.034)
 H01L(0.034) H02H(0.036) H02I(0.035) H02G(0.041) H02J(0.041) H02K(0.033)
 H02L(0.033) H02M(0.038) H02N(0.038) H02O(0.035) H02P(0.035) H02S(0.039)
 H02T(0.05) H02A(0.042) H02B(0.042) H02C(0.038) H02D(0.038) H02E(0.042)
 H02F(0.042) H02Q(0.039) H02R(0.039) H02U(0.045) H02V(0.045) H02W(0.041)
 H02X(0.041) H8AA(0.065) H(0.065) HA(0.065) H9AA(0.039) HB(0.039) H03A(0.037)
 H03B(0.037) H033(0.047) H03V(0.048) H03W(0.048) H035(0.056) H036(0.049)
 H0BA(0.038) HC(0.038) H03C(0.041) H03D(0.041) H039(0.04) H1BA(0.039) HD(0.039)
 H03X(0.046) H03Y(0.046) H2BA(0.036) HE(0.036) H03E(0.041) H03F(0.041)
 H03Z(0.038) HF(0.038) H03(0.049) HG(0.049) H03G(0.057) H03H(0.048) H03I(0.048)
 H3BA(0.043) HH(0.043) H03J(0.047) H0AA(0.049) HI(0.049) H1AA(0.047)
 H03K(0.052) H03L(0.052) H03M(0.047) H03N(0.047) H2AA(0.046) HJ(0.046)
 H3AA(0.06) H03O(0.045) H03P(0.045) H03R(0.049) H4AA(0.054) H03Q(0.055)
 H03S(0.055) H0CA(0.076) HK(0.076) HL(0.076) H5AA(0.04) H1CA(0.054) HM(0.054)
 H6AA(0.054) H03T(0.047) H03U(0.047) H7AA(0.055) H4BA(0.049) HN(0.049)
 H04K(0.044) H04L(0.044) H042(0.056) H043(0.052) H2CA(0.046) HO(0.046)
 H3CA(0.042) HP(0.042) H4CA(0.043) HQ(0.043) H04A(0.062) H04B(0.062) H5BA(0.05)
 HR(0.05) H5CA(0.052) HS(0.052) H04M(0.06) H04P(0.054) H04Q(0.054) H04R(0.068)
 H6CA(0.058) HT(0.058) H7CA(0.067) HU(0.067) HV(0.067) H04S(0.054) H6BA(0.055)
 HW(0.055) H7BA(0.052) HX(0.052) H8BA(0.084) HY(0.084) HZ(0.084) H04C(0.063)
 H04D(0.063) H04N(0.055) H04O(0.056) H04T(0.066) H04U(0.051) H04V(0.051)
 H8CA(0.057) H3DA(0.057) H04E(0.059) H04F(0.059) H04G(0.063) H04H(0.063)
 H04I(0.059) H04J(0.059) H9BA(0.07) H4DA(0.07) H04W(0.065) H04X(0.065)
 H04Y(0.07) H04Z(0.063) H5DA(0.063) H04(0.071) H6DA(0.071) H050(0.066)
 H05A(0.061) H05B(0.061) H05X(0.061) H05Y(0.061) H053(0.065) H054(0.06)
 H05H(0.062) H05K(0.062) H056(0.088) H05C(0.073) H05D(0.073) H9CA(0.077)
 H7DA(0.077) H05L(0.059) H05N(0.059) H05P(0.069) H05Q(0.063) H05R(0.063)
 H05E(0.07) H05Z(0.088) H8DA(0.088) H9DA(0.088) H05F(0.065) H05G(0.063)
 H05S(0.059) H05I(0.086) H05J(0.086) H05(0.143) H0EA(0.143) H1EA(0.143)
 H05T(0.068) H05M(0.072) H05O(0.069) H05U(0.071) H05V(0.087) H05W(0.079)
 H0DA(0.102) H2EA(0.102) H1DA(0.135) H3EA(0.135) H2DA(0.137) H4EA(0.137)
 H5EA(0.137) H06A(0.169) H06B(0.169) H06C(0.169)
 Fixed X: H01G(0.5042) H01H(0.5278) H01A(0.2429) H01B(0.2585) H01I(0.7578)
 H01J(0.7013) H01C(0.0139) H01D(-0.048) H01E(0.0292) H01F(0.0945) H01K(0.3416)
 H01L(0.3912) H02H(0.1657) H02I(0.317) H02G(0.726) H02J(0.7467) H02K(0.2697)
 H02L(0.1854) H02M(0.3525) H02N(0.3213) H02O(0.136) H02P(0.1886) H02S(0.1178)
 H02T(0.3885) H02A(0.2251) H02B(0.2797) H02C(0.2103) H02D(0.1384) H02E(0.3521)
 H02F(0.3566) H02Q(0.002) H02R(0.0233) H02U(0.1672) H02V(0.0919) H02W(0.17)
 H02X(0.2449) H8AA(-0.0658) H(0.0098) HA(-0.0268) H9AA(-0.0357) HB(-0.0092)
 H03A(0.1075) H03B(0.1605) H033(0.1843) H03V(0.5756) H03W(0.6533) H035(0.2581)
 H036(0.3217) H0BA(-0.1749) HC(-0.2034) H03C(0.2882) H03D(0.3179) H039(0.197)
 H1BA(-0.0473) HD(-0.0123) H03X(0.2877) H03Y(0.2146) H2BA(-0.164) HE(-0.1305)
 H03E(0.276) H03F(0.2968) H03Z(0.5461) HF(0.605) H03(0.5739) HG(0.6274)
 H03G(0.4634) H03H(0.4005) H03I(0.4277) H3BA(-0.1087) HH(-0.1434) H03J(0.2507)
 H0AA(0.2044) HI(0.1631) H1AA(0.3003) H03K(0.3) H03L(0.3362) H03M(0.2541)
 H03N(0.1648) H2AA(0.5636) HJ(0.469) H3AA(0.2241) H03O(0.3265) H03P(0.3786)
 H03R(0.3859) H4AA(0.6071) H03Q(0.5245) H03S(0.5633) H0CA(0.0442) HK(0.0784)
 HL(0.0101) H5AA(0.0835) H1CA(0.1689) HM(0.1007) H6AA(0.5079) H03T(0.2171)
 H03U(0.265) H7AA(0.8276) H4BA(-0.128) HN(-0.1734) H04K(0.0813) H04L(0.071)
 H042(0.3976) H043(0.3465) H2CA(0.2813) HO(0.2361) H3CA(0.1193) HP(0.1646)
 H4CA(0.0595) HQ(0.1213) H04A(0.4776) H04B(0.3859) H5BA(-0.2653) HR(-0.2243)
 H5CA(-0.0015) HS(0.0652) H04M(0.3391) H04P(0.5632) H04Q(0.6212) H04R(0.1247)
 H6CA(0.2351) HT(0.3126) H7CA(-0.0476) HU(-0.0494) HV(0.0202) H04S(0.6283)
 H6BA(-0.0434) HW(-0.0965) H7BA(-0.1352) HX(-0.0972) H8BA(-0.1626) HY(-0.2572)
 HZ(-0.2074) H04C(0.3846) H04D(0.2897) H04N(0.4737) H04O(0.5351) H04T(0.6772)
 H04U(0.6804) H04V(0.6983) H8CA(0.3752) H3DA(0.3355) H04E(0.4294) H04F(0.4681)
 H04G(0.523) H04H(0.459) H04I(0.3673) H04J(0.3528) H9BA(0.0636) H4DA(0.0746)
 H04W(0.483) H04X(0.4792) H04Y(0.3648) H04Z(0.6747) H5DA(0.5891) H04(0.7881)
 H6DA(0.7982) H050(0.1581) H05A(-0.0049) H05B(0.0697) H05X(-0.0765) H05Y(-
 0.0594) H053(0.2052) H054(0.3351) H05H(0.7411) H05K(0.7685) H056(0.2302)
 H05C(0.415) H05D(0.4617) H9CA(0.409) H7DA(0.3717) H05L(0.3851) H05N(0.4264)
 H05P(0.1454) H05Q(0.415) H05R(0.3832) H05E(0.0126) H05Z(-0.1569) H8DA(-0.136)
 H9DA(-0.2076) H05F(0.002) H05G(0.1456) H05S(0.5276) H05I(0.0937) H05J(0.2881)
 H05(-0.0033) H0EA(-0.019) H1EA(0.0682) H05T(0.4487) H05M(0.057) H05O(0.2041)
 H05U(0.6594) H05V(0.5774) H05W(0.4751) H0DA(0.354) H2EA(0.2675) H1DA(0.3587)
 H3EA(0.3582) H2DA(0.4702) H4EA(0.5097) H5EA(0.51) H06A(0.2199) H06B(0.2657)
 H06C(0.2171)
 Fixed Y: H01G(-0.2265) H01H(-0.1946) H01A(0.5144) H01B(0.4429) H01I(-0.0055)
 H01J(0.0568) H01C(0.4626) H01D(0.4571) H01E(0.2774) H01F(0.2925) H01K(0.1381)
 H01L(0.0617) H02H(0.5628) H02I(0.38) H02G(0.1764) H02J(0.1837) H02K(0.4478)
 H02L(0.4295) H02M(0.4223) H02N(0.3856) H02O(0.3723) H02P(0.3558) H02S(0.3796)
 H02T(0.3356) H02A(0.1747) H02B(0.224) H02C(0.7357) H02D(0.7615) H02E(0.2766)
 H02F(0.2868) H02Q(0.8614) H02R(0.8998) H02U(0.5307) H02V(0.4986) H02W(0.3747)
 H02X(0.4071) H8AA(1.1418) H(1.0768) HA(1.1492) H9AA(1.0582) HB(0.9841)
 H03A(0.6673) H03B(0.5808) H033(0.3341) H03V(0.3405) H03W(0.2856) H035(0.0206)
 H036(0.3113) H0BA(0.8955) HC(0.9759) H03C(0.7) H03D(0.7065) H039(0.6475)
 H1BA(0.9772) HD(1.0136) H03X(0.5551) H03Y(0.6066) H2BA(1.0341) HE(0.9564)
 H03E(0.5382) H03F(0.5979) H03Z(0.3262) HF(0.2609) H03(0.016) HG(-0.0702)
 H03G(0.5454) H03H(0.5912) H03I(0.5109) H3BA(1.0385) HH(1.11) H03J(0.8001)
 H0AA(0.4641) HI(0.5501) H1AA(0.518) H03K(0.5481) H03L(0.614) H03M(0.7495)
 H03N(0.7708) H2AA(-0.1755) HJ(-0.1563) H3AA(-0.2123) H03O(0.5745) H03P(0.4999)
 H03R(0.5774) H4AA(-0.0335) H03Q(0.4901) H03S(0.5555) H0CA(0.5763) HK(0.6175)
 HL(0.5772) H5AA(0.4707) H1CA(0.4992) HM(0.4575) H6AA(-0.2054) H03T(0.159)
 H03U(0.1995) H7AA(0.2397) H4BA(1.1106) HN(1.0705) H04K(0.5769) H04L(0.508)
 H042(0.7533) H043(0.0919) H2CA(0.4324) HO(0.4979) H3CA(0.459) HP(0.3886)
 H4CA(0.3867) HQ(0.3091) H04A(0.6697) H04B(0.6754) H5BA(0.9077) HR(0.8259)
 H5CA(0.4011) HS(0.3306) H04M(-0.2006) H04P(-0.1356) H04Q(-0.1612) H04R(-
 0.1041) H6CA(0.2787) HT(0.3038) H7CA(0.3189) HU(0.2926) HV(0.248) H04S(0.3814)
 H6BA(1.1276) HW(1.0944) H7BA(0.9259) HX(0.8463) H8BA(0.7869) HY(0.8113)
 HZ(0.8679) H04C(0.0172) H04D(0.0479) H04N(0.1934) H04O(0.5687) H04T(0.4066)
 H04U(0.129) H04V(0.1946) H8CA(0.3837) H3DA(0.4622) H04E(0.1729) H04F(0.0927)
 H04G(0.6824) H04H(0.6972) H04I(0.7078) H04J(0.7013) H9BA(0.7403) H4DA(0.7755)
 H04W(0.0563) H04X(-0.0025) H04Y(0.0128) H04Z(0.4469) H5DA(0.4378) H04(0.2961)
 H6DA(0.3593) H050(-0.072) H05A(0.1153) H05B(0.1344) H05X(0.8) H05Y(0.8409)
 H053(0.0737) H054(0.0669) H05H(0.273) H05K(0.3456) H056(-0.1348) H05C(0.1528)
 H05D(0.081) H9CA(0.453) H7DA(0.5306) H05L(-0.0196) H05N(0.0463) H05P(0.0168)
 H05Q(-0.1108) H05R(-0.1181) H05E(0.0049) H05Z(1.2295) H8DA(1.2292)
 H9DA(1.1972) H05F(0.1334) H05G(0.0755) H05S(0.1691) H05I(-0.1103) H05J(-
 0.0425) H05(0.704) H0EA(0.6712) H1EA(0.6477) H05T(0.2614) H05M(0.0193) H05O(-
 0.0429) H05U(0.3114) H05V(0.4059) H05W(0.3788) H0DA(0.301) H2EA(0.3074)
 H1DA(0.1834) H3EA(0.1758) H2DA(0.4874) H4EA(0.4144) H5EA(0.497) H06A(0.1908)
 H06B(0.1146) H06C(0.1868)
 Fixed Z: H01G(0.5921) H01H(0.6274) H01A(0.9799) H01B(0.9643) H01I(0.5321)
 H01J(0.5038) H01C(0.8396) H01D(0.8804) H01E(1.0806) H01F(1.0456) H01K(0.6328)
 H01L(0.6378) H02H(0.418) H02I(1.072) H02G(0.5434) H02J(0.4831) H02K(0.437)
 H02L(0.4508) H02M(0.3549) H02N(0.3175) H02O(0.3915) H02P(0.3398) H02S(1.1579)
 H02T(1.1426) H02A(0.931) H02B(0.8946) H02C(1.0232) H02D(1.0646) H02E(0.9934)
 H02F(0.9328) H02Q(0.7062) H02R(0.6486) H02U(0.6) H02V(0.6226) H02W(0.6121)
 H02X(0.5913) H8AA(0.471) H(0.4927) HA(0.5181) H9AA(0.6026) HB(0.5784)
 H03A(1.1422) H03B(1.1518) H033(1.2307) H03V(0.4465) H03W(0.4229) H035(0.6138)
 H036(1.2235) H0BA(0.6928) HC(0.7089) H03C(0.7746) H03D(0.8256) H039(1.2039)
 H1BA(0.7356) HD(0.6807) H03X(0.3646) H03Y(0.3325) H2BA(0.6291) HE(0.6096)
 H03E(1.0884) H03F(1.0389) H03Z(0.5424) HF(0.5793) H03(0.7275) HG(0.7329)
 H03G(0.7125) H03H(0.8812) H03I(0.8645) H3BA(0.5216) HH(0.5481) H03J(1.0755)
 H0AA(0.2675) HI(0.2732) H1AA(0.2844) H03K(1.1759) H03L(1.1809) H03M(1.1652)
 H03N(1.1504) H2AA(0.7393) HJ(0.7401) H3AA(0.6966) H03O(0.7486) H03P(0.7833)
 H03R(1.101) H4AA(0.8136) H03Q(0.7914) H03S(0.7587) H0CA(0.4935) HK(0.5262)
 HL(0.5516) H5AA(0.3214) H1CA(0.5211) HM(0.5434) H6AA(0.8258) H03T(1.0267)
 H03U(1.0511) H7AA(0.5138) H4BA(0.6687) HN(0.7182) H04K(0.3544) H04L(0.4005)
 H042(0.7528) H043(0.9031) H2CA(0.711) HO(0.6677) H3CA(0.7011) HP(0.7417)
 H4CA(0.6731) HQ(0.6967) H04A(0.701) H04B(0.6994) H5BA(0.786) HR(0.7727)
 H5CA(0.7532) HS(0.78) H04M(0.6463) H04P(0.8635) H04Q(0.8156) H04R(0.7079)
 H6CA(0.6782) HT(0.6515) H7CA(0.7203) HU(0.781) HV(0.7456) H04S(0.5741)
 H6BA(0.7232) HW(0.7714) H7BA(0.7819) HX(0.7647) H8BA(0.8497) HY(0.8602)
 HZ(0.8631) H04C(0.9841) H04D(0.9865) H04N(0.9639) H04O(0.8442) H04T(0.4181)
 H04U(0.7269) H04V(0.6812) H8CA(0.6417) H3DA(0.6048) H04E(0.8925) H04F(0.928)
 H04G(0.7821) H04H(0.8298) H04I(1.1028) H04J(1.0476) H9BA(0.6811) H4DA(0.6214)
 H04W(0.8021) H04X(0.8555) H04Y(0.8126) H04Z(0.495) H5DA(0.4909) H04(0.4307)
 H6DA(0.4573) H050(1.1275) H05A(0.8776) H05B(0.8411) H05X(0.6792) H05Y(0.6212)
 H053(0.8743) H054(1.0594) H05H(0.5863) H05K(0.5535) H056(0.9681) H05C(1.0469)
 H05D(1.0223) H9CA(0.6938) H7DA(0.6554) H05L(0.7303) H05N(0.7272) H05P(0.6703)
 H05Q(0.8615) H05R(0.8115) H05E(0.9409) H05Z(0.698) H8DA(0.7532) H9DA(0.7479)
 H05F(1.1115) H05G(0.9934) H05S(0.7666) H05I(0.9842) H05J(0.9151) H05(0.6042)
 H0EA(0.6638) H1EA(0.6356) H05T(0.8108) H05M(1.1634) H05O(1.0432) H05U(0.6953)
 H05V(0.7348) H05W(0.7961) H0DA(0.726) H2EA(0.7555) H1DA(0.7755) H3EA(0.7181)
 H2DA(0.5888) H4EA(0.63) H5EA(0.6347) H06A(0.7914) H06B(0.7716) H06C(0.7336)
;
_olex2_submission_special_instructions 'No special instructions were received'