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_7048464
_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
'C104 H72 I8 Mo6 N14 O12 Zn2, 4(C H2 Cl2), 2(C16 H36 N)'
_chemical_formula_sum            'C140 H152 Cl8 I8 Mo6 N16 O12 Zn2'
_chemical_formula_weight         4255.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-04-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_audit_update_record
;
2018-12-17 deposited with the CCDC.
2019-01-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.286(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.9029(7)
_cell_length_b                   21.0461(13)
_cell_length_c                   29.4339(19)
_cell_measurement_reflns_used    19856
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.605
_cell_measurement_theta_min      2.950
_cell_volume                     7371.6(8)
_computing_cell_refinement       'SAINT-Plus (Bruker, 1998)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT-Plus (Bruker, 1998)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'Bruker KAPPA APEX II area-detector diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            66689
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         4.082
_exptl_absorpt_coefficient_mu    2.697
_exptl_absorpt_correction_T_max  0.813
_exptl_absorpt_correction_T_min  0.687
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.917
_exptl_crystal_description       block
_exptl_crystal_F_000             4144
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.137
_refine_diff_density_min         -1.981
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     871
_refine_ls_number_reflns         16876
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0320
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0260P)^2^+25.6363P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0681
_refine_ls_wR_factor_ref         0.0777
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13166
_reflns_number_total             16876
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04452j2.cif
_cod_data_source_block           CP2
_cod_depositor_comments
'Adding full bibliography for 7048462--7048465.cif.'
_cod_database_code               7048464
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.813
_shelx_estimated_absorpt_t_min   0.412
_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.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C2S(H2SA,H2SB), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,
 H43B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B), C61(H61A,H61B),
 C62(H62A,H62B), C63(H63A,H63B), C71(H71A,H71B), C72(H72A,H72B), C73(H73A,H73B)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C22(H22), C23(H23), C24(H24),
 C25(H25), C32(H32), C33(H33), C34(H34), C35(H35), C102(H102), C103(H103),
 C105(H105), C107(H107), C108(H108), C112(H112), C113(H113), C116(H116),
 C117(H117), C119(H119), C120(H120), C122(H122), C124(H124), C125(H125),
 C129(H129), C130(H130), C133(H133), C134(H134)
2.c Idealised Me refined as rotating group:
 C115(H11A,H11B,H11C), C132(H13A,H13B,H13C), C44(H44A,H44B,H44C), C54(H54A,
 H54B,H54C), C64(H64A,H64B,H64C), C74(H74A,H74B,H74C)
;
_shelx_res_checksum              56033
_olex2_submission_special_instructions 'No special instructions were received'