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_7048462
_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         'C18 H12 I4 Mo3 N3 O6, C16 H36 N'
_chemical_formula_sum            'C34 H48 I4 Mo3 N4 O6'
_chemical_formula_weight         1404.18
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2018-01-31
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-04-04 deposited with the CCDC.
2019-01-03 downloaded from the CCDC.
;
_cell_angle_alpha                113.400(2)
_cell_angle_beta                 93.501(2)
_cell_angle_gamma                97.357(2)
_cell_formula_units_Z            2
_cell_length_a                   10.5010(8)
_cell_length_b                   13.9062(11)
_cell_length_c                   16.2223(13)
_cell_measurement_reflns_used    9547
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      33.00
_cell_measurement_theta_min      2.26
_cell_volume                     2139.8(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2008 (Burla et al., 2007)'
_diffrn_ambient_temperature      150.0(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0203
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.902
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            36120
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.902
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         33.019
_diffrn_reflns_theta_min         1.618
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.796
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6181
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0601 before and 0.0348 after correction. The Ratio of minimum to maximum transmission is 0.8280. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.179
_exptl_crystal_description       block
_exptl_crystal_F_000             1332
_exptl_crystal_size_max          0.364
_exptl_crystal_size_mid          0.162
_exptl_crystal_size_min          0.126
_refine_diff_density_max         4.150
_refine_diff_density_min         -2.007
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         14578
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0347
_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^)+(0.0380P)^2^+7.7962P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0842
_refine_ls_wR_factor_ref         0.0923
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11853
_reflns_number_total             14578
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04452j2.cif
_cod_data_source_block           qqq
_cod_depositor_comments
'Adding full bibliography for 7048462--7048465.cif.'
_cod_database_code               7048462
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.646
_shelx_estimated_absorpt_t_min   0.339
_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:
 C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C21(H21A,H21B), C22(H22A,
 H22B), C23(H23A,H23B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B),
 C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B)
2.b Aromatic/amide H refined with riding coordinates:
 C3A(H3A), C3B(H3B), C3C(H3C), C4A(H4A), C4B(H4B), C4C(H4C), C6A(H6A),
 C6B(H6B), C6C(H6C), C7A(H7A), C7B(H7B), C7C(H7C)
2.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C24(H24A,H24B,H24C), C34(H34A,H34B,H34C), C44(H44A,H44B,
 H44C)
;
_shelx_res_checksum              79006
_olex2_submission_special_instructions 'No special instructions were received'