Hybrid organic-inorganic supramolecular systems based on a pyridine end-decorated molybdenum(ii) halide cluster and zinc(ii) porphyrinate.
Volostnykh, Marina V.; Mikhaylov, Maxim A.; Sinelshchikova, Anna A.; Kirakosyan, Gayane A.; Martynov, Alexander G.; Grigoriev, Mikhail S.; Piryazev, Dmitry A.; Tsivadze, Aslan Yu; Sokolov, Maxim N.; Gorbunova, Yulia G.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 1835–1842; doi:10.1039/c8dt04452j

data_7048465
_publ_section_title
;
 Hybrid organic-inorganic supramolecular systems based on a pyridine
 end-decorated molybdenum(ii) halide cluster and zinc(ii) porphyrinate.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1835
_journal_page_last               1842
_journal_paper_doi               10.1039/c8dt04452j
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety
;
C240 H168 I8 Mo6 N30 O12 Zn6, 2(C34 H26 N4 O Zn), 2(C16 H36 N), 4(C H2 Cl2), 4(C6 H14).
;
_chemical_formula_sum            'C368 H356 Cl8 I8 Mo6 N40 O14 Zn8'
_chemical_formula_weight         7960.31
_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
_audit_creation_date             2018-12-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-12-17 deposited with the CCDC.
2019-01-03 downloaded from the CCDC.
;
_cell_angle_alpha                103.620(2)
_cell_angle_beta                 107.057(3)
_cell_angle_gamma                98.424(2)
_cell_formula_units_Z            1
_cell_length_a                   20.2530(10)
_cell_length_b                   20.5959(11)
_cell_length_c                   21.6995(10)
_cell_measurement_reflns_used    5694
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.714
_cell_measurement_theta_min      2.684
_cell_volume                     8180.5(7)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
'Bruker KAPPA APEX II area-detector diffractometer'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1055
_diffrn_reflns_av_unetI/netI     0.1867
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            62272
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         4.085
_exptl_absorpt_coefficient_mu    1.685
_exptl_absorpt_correction_T_max  0.904
_exptl_absorpt_correction_T_min  0.701
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_description       fragment
_exptl_crystal_F_000             4008
_exptl_crystal_recrystallization_method 'CH2Cl2/hexane, ambient temperature'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.758
_refine_diff_density_min         -1.613
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.941
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1932
_refine_ls_number_reflns         28666
_refine_ls_number_restraints     1402
_refine_ls_restrained_S_all      0.921
_refine_ls_R_factor_all          0.1936
_refine_ls_R_factor_gt           0.0717
_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^)+(0.1179P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1719
_refine_ls_wR_factor_ref         0.2503
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11676
_reflns_number_total             28666
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04452j2.cif
_cod_data_source_block           cp6_sq
_cod_depositor_comments
'Adding full bibliography for 7048462--7048465.cif.'
_cod_database_code               7048465
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.906
_shelx_estimated_absorpt_t_min   0.552
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H31A(0.788) H31B(0.788) H31C(0.788) H12(0.059) H13(0.065)
 H14(0.067) H15(0.063) H22(0.067) H23(0.067) H24(0.07) H25(0.062) H32(0.098)
 H33(0.099) H34(0.089) H35(0.073) H102(0.089) H103(0.089) H105(0.089)
 H107(0.105) H108(0.095) H112(0.107) H113(0.135) H11A(0.133) H11B(0.133)
 H11C(0.133) H116(0.101) H117(0.097) H119(0.072) H120(0.072) H122(0.071)
 H124(0.081) H125(0.08) H129(0.094) H130(0.109) H13A(0.207) H13B(0.207)
 H13C(0.207) H133(0.112) H134(0.101) H202(0.081) H203(0.077) H205(0.08)
 H207(0.088) H208(0.089) H212(0.167) H213(0.19) H21A(0.216) H21B(0.216)
 H21C(0.216) H216(0.26) H217(0.207) H219(0.132) H220(0.139) H222(0.108)
 H224(0.113) H225(0.106) H229(0.113) H230(0.134) H23A(0.286) H23B(0.286)
 H23C(0.286) H233(0.177) H234(0.147) H302(0.099) H303(0.102) H305(0.107)
 H307(0.151) H308(0.164) H317(0.52) H316(0.781) H313(0.293) H312(0.244)
 H319(0.228) H320(0.216) H322(0.119) H324(0.098) H325(0.095) H329(0.092)
 H330(0.094) H33A(0.162) H33B(0.162) H33C(0.162) H333(0.094) H334(0.089)
 H41A(0.07) H41B(0.07) H402(0.099) H403(0.089) H405(0.087) H407(0.078)
 H408(0.07) H412(0.074) H413(0.069) H41C(0.104) H41D(0.104) H41E(0.104)
 H416(0.07) H417(0.068) H419(0.063) H420(0.064) H422(0.064) H424(0.071)
 H425(0.074) H429(0.122) H430(0.135) H43A(0.185) H43B(0.185) H43C(0.185)
 H433(0.1) H434(0.103) H1SA(0.085) H1SB(0.085) H2SA(0.187) H2SB(0.187)
 H51A(0.097) H51B(0.097) H52A(0.114) H52B(0.114) H53A(0.091) H53B(0.091)
 H54A(0.162) H54B(0.162) H54C(0.162) H61A(0.092) H61B(0.092) H62A(0.129)
 H62B(0.129) H63A(0.137) H63B(0.137) H64A(0.37) H64B(0.37) H64C(0.37)
 H71A(0.09) H71B(0.09) H72A(0.091) H72B(0.091) H73A(0.089) H73B(0.089)
 H74A(0.139) H74B(0.139) H74C(0.139) H81A(0.101) H81B(0.101) H82A(0.09)
 H82B(0.09) H83A(0.108) H83B(0.108) H84A(0.162) H84B(0.162) H84C(0.162)
 Fixed X: H31A(1.044) H31B(1.0847) H31C(1.078) H12(0.2419) H13(0.142)
 H14(0.0921) H15(0.1938) H22(0.6917) H23(0.7324) H24(0.7099) H25(0.6705)
 H32(0.5988) H33(0.6539) H34(0.4962) H35(0.4371) H102(0.0568) H103(-0.0274)
 H105(-0.0994) H107(-0.1596) H108(-0.1522) H112(-0.1696) H113(-0.1961) H11A(-
 0.1675) H11B(-0.0882) H11C(-0.1506) H116(-0.0341) H117(-0.0046) H119(-0.0151)
 H120(0.0572) H122(0.1023) H124(0.1584) H125(0.1656) H129(0.2287) H130(0.299)
 H13A(0.3127) H13B(0.2457) H13C(0.2695) H133(0.1243) H134(0.0516) H202(0.7154)
 H203(0.6043) H205(0.5652) H207(0.5139) H208(0.561) H212(0.7263) H213(0.6974)
 H21A(0.5648) H21B(0.5724) H21C(0.6367) H216(0.5731) H217(0.5968) H219(0.8116)
 H220(0.9218) H222(0.9663) H224(1.0138) H225(0.9672) H229(0.8468) H230(0.8748)
 H23A(0.8779) H23B(0.958) H23C(0.903) H233(0.8933) H234(0.8553) H302(0.5189)
 H303(0.6241) H305(0.7303) H307(0.8354) H308(0.8783) H317(0.8162) H316(0.9183)
 H313(1.0363) H312(0.9342) H319(0.7949) H320(0.6897) H322(0.5754) H324(0.4657)
 H325(0.4189) H329(0.4605) H330(0.3611) H33A(0.2227) H33B(0.2487) H33C(0.2732)
 H333(0.3086) H334(0.4046) H402(0.3331) H403(0.4536) H405(0.523) H407(0.5955)
 H408(0.5649) H412(0.5258) H413(0.5768) H41C(0.5876) H41D(0.5575) H41E(0.5089)
 H416(0.4466) H417(0.3982) H419(0.3211) H420(0.1975) H422(0.1302) H424(0.0589)
 H425(0.0908) H429(0.1835) H430(0.1114) H43A(0.0409) H43B(0.0514) H43C(0.1063)
 H433(0.1379) H434(0.2022) H1SA(0.3576) H1SB(0.2835) H2SA(0.3625) H2SB(0.3964)
 H51A(0.225) H51B(0.1503) H52A(0.2805) H52B(0.2049) H53A(0.2877) H53B(0.2061)
 H54A(0.2319) H54B(0.3134) H54C(0.2796) H61A(0.1937) H61B(0.1559) H62A(0.0502)
 H62B(0.0883) H63A(0.1018) H63B(0.021) H64A(0.0159) H64B(0.0872) H64C(0.0151)
 H71A(0.2859) H71B(0.2893) H72A(0.2354) H72B(0.2322) H73A(0.3587) H73B(0.3624)
 H74A(0.3824) H74B(0.3042) H74C(0.3147) H81A(0.1312) H81B(0.0925) H82A(0.1529)
 H82B(0.2111) H83A(0.1332) H83B(0.067) H84A(0.0965) H84B(0.1728) H84C(0.1025)
 Fixed Y: H31A(0.913) H31B(0.988) H31C(0.929) H12(0.3496) H13(0.2869)
 H14(0.4557) H15(0.5226) H22(0.4169) H23(0.4642) H24(0.6459) H25(0.6039)
 H32(0.8002) H33(0.9152) H34(0.9601) H35(0.8464) H102(0.0875) H103(0.1262)
 H105(0.2217) H107(0.334) H108(0.4344) H112(0.4938) H113(0.6001) H11A(0.712)
 H11B(0.7448) H11C(0.7216) H116(0.6579) H117(0.5532) H119(0.532) H120(0.4836)
 H122(0.3698) H124(0.2625) H125(0.1661) H129(0.1788) H130(0.0991) H13A(-0.0143)
 H13B(-0.0763) H13C(-0.056) H133(-0.0547) H134(0.0232) H202(0.3488)
 H203(0.3847) H205(0.4993) H207(0.6112) H208(0.728) H212(0.8657) H213(0.9666)
 H21A(1.0016) H21B(0.9926) H21C(1.0385) H216(0.884) H217(0.7806) H219(0.8555)
 H220(0.8159) H222(0.7079) H224(0.5967) H225(0.478) H229(0.3803) H230(0.2751)
 H23A(0.1589) H23B(0.1988) H23C(0.1767) H233(0.2694) H234(0.3731) H302(1.1383)
 H303(1.1066) H305(1.0566) H307(1.0018) H308(0.983) H317(0.9014) H316(0.8723)
 H313(1.0583) H312(1.0874) H319(1.0193) H320(1.0432) H322(1.076) H324(1.1186)
 H325(1.1342) H329(1.2365) H330(1.2689) H33A(1.1902) H33B(1.1739) H33C(1.2497)
 H333(1.0897) H334(1.0552) H402(0.9697) H403(0.9572) H405(0.8557) H407(0.7634)
 H408(0.6428) H412(0.5804) H413(0.4894) H41C(0.3747) H41D(0.3385) H41E(0.327)
 H416(0.3752) H417(0.4674) H419(0.4718) H420(0.4809) H422(0.5763) H424(0.6723)
 H425(0.7913) H429(0.8991) H430(0.9825) H43A(1.0459) H43B(1.0623) H43C(1.105)
 H433(1.0119) H434(0.9241) H1SA(0.3546) H1SB(0.3134) H2SA(0.7307) H2SB(0.8092)
 H51A(0.6538) H51B(0.6715) H52A(0.7742) H52B(0.7848) H53A(0.703) H53B(0.6957)
 H54A(0.8101) H54B(0.8182) H54C(0.7677) H61A(0.808) H61B(0.7768) H62A(0.7285)
 H62B(0.761) H63A(0.8737) H63B(0.8359) H64A(0.7718) H64B(0.8264) H64C(0.8511)
 H71A(0.6829) H71B(0.7633) H72A(0.6754) H72B(0.7546) H73A(0.7877) H73B(0.7087)
 H74A(0.7599) H74B(0.7735) H74C(0.6965) H81A(0.6559) H81B(0.6389) H82A(0.5577)
 H82B(0.5845) H83A(0.5408) H83B(0.5275) H84A(0.4315) H84B(0.4493) H84C(0.4243)
 Fixed Z: H31A(0.4778) H31B(0.489) H31C(0.4252) H12(0.0378) H13(0.0481)
 H14(0.1254) H15(0.1212) H22(0.3117) H23(0.4285) H24(0.4092) H25(0.2923)
 H32(0.094) H33(0.1354) H34(0.1902) H35(0.1549) H102(-0.0439) H103(-0.1276)
 H105(-0.1166) H107(-0.1154) H108(-0.0277) H112(0.1347) H113(0.1396)
 H11A(0.0811) H11B(0.1328) H11C(0.1599) H116(0.0818) H117(0.0777) H119(0.2374)
 H120(0.3234) H122(0.3174) H124(0.3156) H125(0.2263) H129(0.1344) H130(0.126)
 H13A(0.0886) H13B(0.0431) H13C(0.1236) H133(0.0424) H134(0.0498) H202(0.545)
 H203(0.5487) H205(0.5564) H207(0.553) H208(0.5522) H212(0.6414) H213(0.6347)
 H21A(0.5624) H21B(0.4897) H21C(0.5561) H216(0.4497) H217(0.4547) H219(0.5411)
 H220(0.5456) H222(0.5496) H224(0.5501) H225(0.5458) H229(0.4422) H230(0.4192)
 H23A(0.509) H23B(0.5257) H23C(0.4503) H233(0.6091) H234(0.626) H302(0.0191)
 H303(-0.0046) H305(0.0569) H307(0.1125) H308(0.2255) H317(0.3432) H316(0.403)
 H313(0.4244) H312(0.3645) H319(0.442) H320(0.4632) H322(0.3936) H324(0.3333)
 H325(0.2217) H329(0.1711) H330(0.1075) H33A(0.0059) H33B(-0.0578) H33C(-
 0.0062) H333(-0.0364) H334(0.0243) H402(0.2772) H403(0.2916) H405(0.3063)
 H407(0.3266) H408(0.3258) H412(0.3991) H413(0.414) H41C(0.374) H41D(0.2943)
 H41E(0.3389) H416(0.2274) H417(0.2128) H419(0.2944) H420(0.2701) H422(0.2482)
 H424(0.2388) H425(0.2428) H429(0.3591) H430(0.3566) H43A(0.3011) H43B(0.2356)
 H43C(0.309) H433(0.191) H434(0.1845) H1SA(0.3086) H1SB(0.3075) H2SA(0.4001)
 H2SB(0.4083) H51A(-0.1306) H51B(-0.1332) H52A(-0.0731) H52B(-0.0689) H53A(-
 0.0064) H53B(-0.0127) H54A(0.0535) H54B(0.0592) H54C(0.0936) H61A(-0.1672)
 H61B(-0.2467) H62A(-0.2302) H62B(-0.1504) H63A(-0.1722) H63B(-0.1845) H64A(-
 0.3046) H64B(-0.2912) H64C(-0.2952) H71A(-0.1967) H71B(-0.1752) H72A(-0.3118)
 H72B(-0.2923) H73A(-0.2484) H73B(-0.2666) H74A(-0.3488) H74B(-0.366) H74C(-
 0.3819) H81A(-0.2992) H81B(-0.2486) H82A(-0.2278) H82B(-0.2581) H83A(-0.3663)
 H83B(-0.3416) H84A(-0.3138) H84B(-0.3214) H84C(-0.3869)
;
_shelx_res_checksum              90950
_shelx_fab_checksum              51029
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'