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_7048879
_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
'C74 H118 Co6 Mo10 N2 O58 P6, 9.5(C2 H3 N), 2(C16 H36 N)'
_chemical_formula_sum            'C125 H218.5 Co6 Mo10 N13.5 O58 P6'
_chemical_formula_weight         4337.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-08-30
_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                90
_cell_angle_beta                 107.6720(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.6667(8)
_cell_length_b                   25.3666(12)
_cell_length_c                   20.0291(9)
_cell_measurement_reflns_used    9914
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.90
_cell_measurement_theta_min      2.28
_cell_volume                     8552.3(7)
_computing_cell_refinement       'SAINT V8.35A (?, 2016)'
_computing_data_reduction        'SAINT V8.35A (?, 2016)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_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  0.0909
_diffrn_reflns_av_unetI/netI     0.0967
_diffrn_reflns_Laue_measured_fraction_full 1.000
_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       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            104339
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.117
_diffrn_reflns_theta_min         1.335
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.409
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6590
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0612 before and 0.0545 after correction. The Ratio of minimum to maximum transmission is 0.8840. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.684
_exptl_crystal_description       block
_exptl_crystal_F_000             4398
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.042
_refine_diff_density_min         -1.222
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.889
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1006
_refine_ls_number_reflns         16945
_refine_ls_number_restraints     83
_refine_ls_restrained_S_all      0.892
_refine_ls_R_factor_all          0.0817
_refine_ls_R_factor_gt           0.0356
_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^)+(0.0266P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0643
_refine_ls_wR_factor_ref         0.0730
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10513
_reflns_number_total             16945
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00075e2.cif
_cod_data_source_block           pw015_a
_cod_depositor_comments
'Adding full bibliography for 7048870--7048879.cif.'
_cod_original_formula_sum        'C125 H218.50 Co6 Mo10 N13.50 O58 P6'
_cod_database_code               7048879
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.933
_shelx_estimated_absorpt_t_min   0.816
_olex2_refinement_description
;
1. Others
 Fixed Sof: N1C(0.25) C1C(0.25) H1CA(0.25) H1CB(0.25) H1CC(0.25) C2C(0.25)
 C1A(0.25) H1AA(0.25) H1AB(0.25) H1AC(0.25) C2A(0.25) C1(0.75) H1A(0.75)
 H1B(0.75) H1C(0.75) C2(0.75) N1(0.5) C1(0.5) H1A(0.5) H1B(0.5) H1C(0.5) C2(0.5)
 Fixed Uiso: H1A(0.031) H1B(0.031) H5A(0.031) H5B(0.031) H23A(0.029)
 H23B(0.029) H3(0.054) H4(0.079) H5(0.077) H6(0.062) H7(0.045) H9A(0.026)
 H9B(0.026) H10(0.032) H11A(0.04) H11B(0.04) H12(0.034) H13A(0.029) H13B(0.029)
 H14A(0.034) H14B(0.034) H15(0.029) H16A(0.033) H16B(0.033) H17A(0.023)
 H17B(0.023) H19A(0.026) H19B(0.026) H20(0.039) H21A(0.047) H21B(0.047)
 H22(0.043) H23C(0.029) H23D(0.029) H24A(0.057) H24B(0.057) H25(0.045)
 H26A(0.031) H26B(0.031) H27A(0.047) H27B(0.047) H29A(0.034) H29B(0.034)
 H30(0.05) H31A(0.064) H31B(0.064) H32(0.052) H33A(0.042) H33B(0.042)
 H34(0.032) H35A(0.04) H35B(0.04) H36A(0.042) H36B(0.042) H37A(0.027)
 H37B(0.027) H55A(0.069) H55B(0.069) H55C(0.069) H1BA(0.111) H1BB(0.111)
 H1BC(0.111) H1CA(0.179) H1CB(0.179) H1CC(0.179) H38A(0.044) H38B(0.044)
 H39A(0.087) H39B(0.087) H40A(0.133) H40B(0.133) H41A(0.303) H41B(0.303)
 H41C(0.303) H42A(0.035) H42B(0.035) H43A(0.038) H43B(0.038) H44A(0.041)
 H44B(0.041) H45A(0.075) H45B(0.075) H45C(0.075) H46A(0.039) H46B(0.039)
 H47A(0.046) H47B(0.046) H48A(0.039) H48B(0.039) H49A(0.061) H49B(0.061)
 H49C(0.061) H50A(0.033) H50B(0.033) H51A(0.03) H51B(0.03) H52A(0.031)
 H52B(0.031) H53A(0.049) H53B(0.049) H53C(0.049) H1AA(0.138) H1AB(0.138)
 H1AC(0.138) H1A(0.111) H1B(0.111) H1C(0.111) H1A(0.138) H1B(0.138) H1C(0.138)
 H1A(0.072) H1B(0.072) H1C(0.072) H1A(0.111) H1B(0.111) H1C(0.111) H1A(0.179)
 H1B(0.179) H1C(0.179)
 Fixed X: H1A(0.703) H1B(0.6593) H5A(0.5697) H5B(0.6505) H23A(0.5993)
 H23B(0.6203) H3(0.4685) H4(0.4265) H5(0.4627) H6(0.5391) H7(0.5772)
 H9A(0.7521) H9B(0.8102) H10(0.8719) H11A(0.9946) H11B(0.9586) H12(1.0023)
 H13A(0.8828) H13B(0.8906) H14A(0.9821) H14B(0.9384) H15(0.8517) H16A(0.8074)
 H16B(0.9017) H17A(0.7901) H17B(0.7401) H19A(0.7398) H19B(0.6647) H20(0.7695)
 H21A(0.8311) H21B(0.8156) H22(0.7721) H23C(0.7419) H23D(0.6677) H24A(0.6403)
 H24B(0.6978) H25(0.5782) H26A(0.5485) H26B(0.5464) H27A(0.6964) H27B(0.6382)
 H29A(0.3108) H29B(0.2283) H30(0.2066) H31A(0.1005) H31B(0.102) H32(0.0875)
 H33A(0.1935) H33B(0.1591) H34(0.3004) H35A(0.3135) H35B(0.2325) H36A(0.1539)
 H36B(0.1907) H37A(0.3221) H37B(0.3682) H55A(0.9542) H55B(0.9153) H55C(0.9522)
 H1BA(0.314) H1BB(0.2731) H1BC(0.2517) H1CA(0.561) H1CB(0.63) H1CC(0.6519)
 H38A(0.4946) H38B(0.4413) H39A(0.5251) H39B(0.5747) H40A(0.4715) H40B(0.4078)
 H41A(0.4576) H41B(0.4223) H41C(0.5164) H42A(0.6546) H42B(0.6649) H43A(0.6251)
 H43B(0.6136) H44A(0.7635) H44B(0.7506) H45A(0.7195) H45B(0.8056) H45C(0.7306)
 H46A(0.5813) H46B(0.5867) H47A(0.4424) H47B(0.4459) H48A(0.521) H48B(0.5156)
 H49A(0.3817) H49B(0.3755) H49C(0.4187) H50A(0.5077) H50B(0.4571) H51A(0.6085)
 H51B(0.5625) H52A(0.4558) H52B(0.4976) H53A(0.6003) H53B(0.5618) H53C(0.5164)
 H1AA(0.513) H1AB(0.4194) H1AC(0.4608) H1A(0.2498) H1B(0.1774) H1C(0.2491)
 H1A(0.523) H1B(0.5968) H1C(0.5621) H1A(0.7203) H1B(0.7206) H1C(0.7166)
 H1A(0.3139) H1B(0.3583) H1C(0.2817) H1A(0.7438) H1B(0.6973) H1C(0.7092)
 Fixed Y: H1A(0.5971) H1B(0.5775) H5A(0.5125) H5B(0.5) H23A(0.33) H23B(0.3654)
 H3(0.3277) H4(0.2618) H5(0.2691) H6(0.339) H7(0.4015) H9A(0.3747) H9B(0.4246)
 H10(0.3494) H11A(0.353) H11B(0.4113) H12(0.3964) H13A(0.4222) H13B(0.4538)
 H14A(0.3034) H14B(0.3307) H15(0.2687) H16A(0.2839) H16B(0.2745) H17A(0.3439)
 H17B(0.3256) H19A(0.4451) H19B(0.4178) H20(0.4269) H21A(0.5023) H21B(0.5123)
 H22(0.5881) H23C(0.5426) H23D(0.5784) H24A(0.594) H24B(0.5685) H25(0.5179)
 H26A(0.5365) H26B(0.4741) H27A(0.4699) H27B(0.4331) H29A(0.3956) H29B(0.4149)
 H30(0.3851) H31A(0.3709) H31B(0.3246) H32(0.2874) H33A(0.2258) H33B(0.2362)
 H34(0.2401) H35A(0.3231) H35B(0.295) H36A(0.3548) H36B(0.2984) H37A(0.2696)
 H37B(0.3076) H55A(0.3885) H55B(0.3801) H55C(0.4361) H1BA(0.5415) H1BB(0.4998)
 H1BC(0.5611) H1CA(0.1035) H1CB(0.0915) H1CC(0.1025) H38A(0.1522) H38B(0.1135)
 H39A(0.0418) H39B(0.0812) H40A(0.0303) H40B(0.0654) H41A(0.1392) H41B(0.097)
 H41C(0.1021) H42A(0.1123) H42B(0.1477) H43A(0.2232) H43B(0.1878) H44A(0.1988)
 H44B(0.1676) H45A(0.2476) H45B(0.2518) H45C(0.2791) H46A(0.054) H46B(0.0916)
 H47A(0.05) H47B(0.0895) H48A(-0.012) H48B(0.0269) H49A(-0.0232) H49B(0.0164)
 H49C(-0.0394) H50A(0.2068) H50B(0.1669) H51A(0.2087) H51B(0.1655) H52A(0.2247)
 H52B(0.2675) H53A(0.2786) H53B(0.2341) H53C(0.2889) H1AA(0.3196) H1AB(0.3092)
 H1AC(0.3493) H1A(0.1944) H1B(0.1584) H1C(0.1326) H1A(0.4103) H1B(0.4182)
 H1C(0.3604) H1A(0.3258) H1B(0.3219) H1C(0.2694) H1A(0.5058) H1B(0.5431)
 H1C(0.5642) H1A(0.1914) H1B(0.1372) H1C(0.1783)
 Fixed Z: H1A(0.6345) H1B(0.6697) H5A(0.3203) H5B(0.3661) H23A(0.575)
 H23B(0.5218) H3(0.3781) H4(0.2928) H5(0.1904) H6(0.1759) H7(0.2636)
 H9A(0.3943) H9B(0.4039) H10(0.3711) H11A(0.463) H11B(0.4468) H12(0.5694)
 H13A(0.5933) H13B(0.5263) H14A(0.5681) H14B(0.6186) H15(0.5443) H16A(0.421)
 H16B(0.4467) H17A(0.577) H17B(0.4995) H19A(0.819) H19B(0.8339) H20(0.9416)
 H21A(0.9098) H21B(0.9837) H22(0.9098) H23C(0.8001) H23D(0.8019) H24A(0.9179)
 H24B(0.9883) H25(0.9491) H26A(0.8262) H26B(0.838) H27A(1.0076) H27B(0.949)
 H29A(0.7806) H29B(0.7269) H30(0.8324) H31A(0.7275) H31B(0.7824) H32(0.67)
 H33A(0.7036) H33B(0.768) H34(0.8077) H35A(0.8659) H35B(0.867) H36A(0.6256)
 H36B(0.6165) H37A(0.7019) H37B(0.7652) H55A(0.7525) H55B(0.8142) H55C(0.8043)
 H1BA(0.7367) H1BB(0.7749) H1BC(0.7749) H1CA(0.4058) H1CB(0.4772) H1CC(0.4065)
 H38A(0.6278) H38B(0.6576) H39A(0.6485) H39B(0.6151) H40A(0.5304) H40B(0.5524)
 H41A(0.5136) H41B(0.4528) H41C(0.4876) H42A(0.7136) H42B(0.7817) H43A(0.7104)
 H43B(0.6417) H44A(0.7491) H44B(0.677) H45A(0.6139) H45B(0.6706) H45C(0.6855)
 H46A(0.7592) H46B(0.8244) H47A(0.7329) H47B(0.7961) H48A(0.817) H48B(0.8784)
 H49A(0.7819) H49B(0.8422) H49C(0.8625) H50A(0.7247) H50B(0.7557) H51A(0.8321)
 H51B(0.8636) H52A(0.8519) H52B(0.8161) H53A(0.9226) H53B(0.9588) H53C(0.9355)
 H1AA(1.0318) H1AB(1.011) H1AC(1.0731) H1A(0.5591) H1B(0.5644) H1C(0.5425)
 H1A(1.0923) H1B(1.0626) H1C(1.0665) H1A(0.8046) H1B(0.8844) H1C(0.8392)
 H1A(0.764) H1B(0.8284) H1C(0.7687) H1A(0.4923) H1B(0.4926) H1C(0.5556)
;
_olex2_submission_special_instructions 'No special instructions were received'