Synthesis, structures and luminescence of several coordination complexes based on β-octamolybdate and Ag/Cu phosphine units
Yu, Yi-Qi; Sun, Shang-Bin; Deng, Wen-Hao; Li, Jian; Lu, Zhi-Yi; He, Jia-Hui; Wang, Long-Sheng; Meng, Xiang-Gao; CrystEngComm 26 (2024) 4329–4338; doi:10.1039/D4CE00496E

data_7249037
_publ_section_title
;
 Synthesis, structures and luminescence of several coordination complexes
 based on \b-octamolybdate and Ag/Cu phosphine units
;
_journal_issue                   32
_journal_name_full               CrystEngComm
_journal_page_first              4329
_journal_page_last               4338
_journal_paper_doi               10.1039/D4CE00496E
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety
'C104.394 H94.789 Cl0.789 Cu4 Mo8 N2 O26 P8, 2(C2 H3 N), 1.606(C H2 Cl2)'
_chemical_formula_sum            'C110 H104 Cl4 Cu4 Mo8 N4 O26 P8'
_chemical_formula_weight         3309.21
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-06-23
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2024-07-01 deposited with the CCDC.	2024-07-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.28(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.265(3)
_cell_length_b                   21.934(4)
_cell_length_c                   23.266(5)
_cell_measurement_reflns_used    5351
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      25.030
_cell_measurement_theta_min      2.303
_cell_volume                     6768(2)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0549
_diffrn_reflns_av_unetI/netI     0.0610
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            37944
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.049
_diffrn_reflns_theta_min         1.857
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.565
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_description       block
_exptl_crystal_F_000             3280
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.610
_refine_diff_density_min         -1.536
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     751
_refine_ls_number_reflns         11941
_refine_ls_number_restraints     297
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0789
_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^)+(0.0685P)^2^+113.9714P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1871
_refine_ls_wR_factor_ref         0.1954
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9426
_reflns_number_total             11941
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00496e2.cif
_cod_data_source_block           b
_cod_depositor_comments
'Adding full bibliography for 7249036--7249039.cif.'
_cod_database_code               7249037
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.766
_shelx_estimated_absorpt_t_min   0.715
_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. Shared sites
{C1S, C1S'}
{Cl1, Cl1'}
3. Rigid bond restraints
 C51, C52, C53, C54, C55, C56
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C61, C62, C63, C64, C65, C66
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C71, C72, C73, C74, C75, C76
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1S', Cl1', Cl2'
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65 \\sim C66: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
C71 \\sim C72 \\sim C73 \\sim C74 \\sim C75 \\sim C76: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
C1S' \\sim Cl1' \\sim Cl2': within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
Uanis(C51) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C54)
\\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C56) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
Uanis(C61) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C64)
\\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C66) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
Uanis(C71) \\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(C74)
\\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(C76) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
Uanis(C1S') \\sim Ueq, Uanis(Cl1') \\sim Ueq, Uanis(Cl2') \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(O9) \\sim Ueq, Uanis(C41) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C1S) = Uanis(C1S')
Uanis(Cl1) = Uanis(Cl1')
5. Others
 Sof(C1S')=Sof(H1SA)=Sof(H1SB)=Sof(Cl1')=Sof(Cl2')=1-FVAR(1)
 Sof(C1S)=Sof(H1SC)=Sof(H1SD)=Sof(Cl1)=Sof(Cl2)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C1S(H1SC,H1SD), C1S'(H1SA,H1SB)
6.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C22(H22), C23(H23),
 C24(H24), C25(H25), C26(H26), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36),
  C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C52(H52), C53(H53),
 C54(H54), C55(H55), C56(H56), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66),
  C72(H72), C73(H73), C74(H74), C75(H75), C76(H76), C82(H82), C83(H83),
 C84(H84), C85(H85), C86(H86)
6.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C3S(H3SA,H3SB,H3SC)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              29522
_shelx_fab_checksum              21376
_olex2_submission_special_instructions 'No special instructions were received'