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_7048463
_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         'C34 H24 N4 Zn'
_chemical_formula_sum            'C34 H24 N4 Zn'
_chemical_formula_weight         553.94
_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             2018-12-15
_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                90
_cell_angle_beta                 93.363(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.9605(15)
_cell_length_b                   9.7595(11)
_cell_length_c                   8.5421(9)
_cell_measurement_reflns_used    4265
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.857
_cell_measurement_theta_min      3.173
_cell_volume                     1245.1(2)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.986
_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  0.0757
_diffrn_reflns_av_unetI/netI     0.0709
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            12363
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.045
_diffrn_reflns_theta_min         4.093
_exptl_absorpt_coefficient_mu    1.019
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.657
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_description       plate
_exptl_crystal_F_000             572
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.240
_refine_diff_density_min         -0.764
_refine_diff_density_rms         0.117
_refine_ls_extinction_coef       0.0052(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2980
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0920
_refine_ls_R_factor_gt           0.0713
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0395P)^2^+8.0074P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1641
_refine_ls_wR_factor_ref         0.1751
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2352
_reflns_number_total             2980
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04452j2.cif
_cod_data_source_block           zndtolp
_cod_depositor_comments
'Adding full bibliography for 7048462--7048465.cif.'
_cod_database_code               7048463
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.95
_shelx_estimated_absorpt_t_min   0.607
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.885(3)
 0.115(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Rigid body (RIGU) restrains
 N2, C6, C5, C4, N1, C1, C2, C3, C7, C8, C9, C10
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C7(H7), C8(H8), C12(H12), C13(H13), C15(H15), C16(H16)
4.b Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C)
;
_shelx_res_checksum              65176
_olex2_submission_special_instructions 'No special instructions were received'