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_7249036
_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         'C108 H90 Ag4 Mo8 O26 P6, 6(C3 H7 N O)'
_chemical_formula_sum            'C126 H132 Ag4 Mo8 N6 O32 P6'
_chemical_formula_weight         3627.19
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-02-29
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2024-05-16 deposited with the CCDC.	2024-07-03 downloaded from the CCDC.
;
_cell_angle_alpha                106.8400(10)
_cell_angle_beta                 92.6010(10)
_cell_angle_gamma                97.4600(10)
_cell_formula_units_Z            1
_cell_length_a                   13.0333(5)
_cell_length_b                   15.0730(6)
_cell_length_c                   18.2889(7)
_cell_measurement_reflns_used    9945
_cell_measurement_temperature    200.00
_cell_measurement_theta_max      72.20
_cell_measurement_theta_min      3.96
_cell_volume                     3396.6(2)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200.00
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.793
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_unetI/netI     0.0557
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.793
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            48101
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.793
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.367
_diffrn_reflns_theta_min         2.047
_diffrn_source_current           3.56
_diffrn_source_power             0.24902200000000002
_diffrn_source_voltage           69.95
_exptl_absorpt_coefficient_mu    1.419
_exptl_absorpt_correction_T_max  0.736
_exptl_absorpt_correction_T_min  0.667
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'blessing, Acta Cryst. 1995(A51) 33-38'
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.773
_exptl_crystal_description       block
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.734
_refine_diff_density_min         -1.293
_refine_diff_density_rms         0.141
_refine_ls_extinction_coef       0.00802(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     917
_refine_ls_number_reflns         16250
_refine_ls_number_restraints     282
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0668P)^2^+2.6037P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1161
_refine_ls_wR_factor_ref         0.1200
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14127
_reflns_number_total             16250
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00496e2.cif
_cod_data_source_block           w
_cod_depositor_comments
'Adding full bibliography for 7249036--7249039.cif.'
_cod_database_code               7249036
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.736
_shelx_estimated_absorpt_t_min   0.667
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1S-C1S = N1S-C2S = N1S-C3S
 1.45 with sigma of 0.01
 N2S-C4S = N2S-C5S = N2S-C6S
 1.45 with sigma of 0.01
 N2S'-C4S' = N2S'-C5S' = N2S'-C6S'
 1.45 with sigma of 0.01
 N3S-C8S = N3S-C9S = N3S-C7S
 1.45 with sigma of 0.01
 N3S'-C8S' = N3S'-C9S' = N3S'-C7S'
 1.45 with sigma of 0.01
 C1S-O1S = C4S-O2S = C4S'-O2S' = C7S-O3S = C7S'-O3S'
 1.2 with sigma of 0.01
 N1S-O1S = N3S-O3S = N2S-O2S = N2S'-O2S' = N3S'-O3S'
 2.1 with sigma of 0.01
 C7S'-C8S' \\sim C7S'-C9S' \\sim C8S'-C9S'
 with sigma of 0.01
3. Restrained planarity
 N3S, O3S, C7S, C8S, C9S
 with sigma of 0.1
 N3S', O3S', C7S', C8S', C9S'
 with sigma of 0.1
4. Rigid bond restraints
 N2S, O2S, C4S, C5S, C6S
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N2S', O2S', C4S', C5S', C6S'
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N3S, O3S, C7S, C8S, C9S
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N3S', O3S', C7S', C8S', C9S'
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
N2S \\sim O2S \\sim C4S \\sim C5S \\sim C6S: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
N2S' \\sim O2S' \\sim C4S' \\sim C5S' \\sim C6S': within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
N3S \\sim O3S \\sim C7S \\sim C8S \\sim C9S: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
N3S' \\sim O3S' \\sim C7S' \\sim C8S' \\sim C9S': within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
Uanis(N2S) \\sim Ueq, Uanis(O2S) \\sim Ueq, Uanis(C4S) \\sim Ueq, Uanis(C5S)
\\sim Ueq, Uanis(C6S) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(N2S') \\sim Ueq, Uanis(O2S') \\sim Ueq, Uanis(C4S') \\sim Ueq,
Uanis(C5S') \\sim Ueq, Uanis(C6S') \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N3S) \\sim Ueq, Uanis(O3S) \\sim Ueq, Uanis(C7S) \\sim Ueq, Uanis(C8S)
\\sim Ueq, Uanis(C9S) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(N3S') \\sim Ueq, Uanis(O3S') \\sim Ueq, Uanis(C7S') \\sim Ueq,
Uanis(C8S') \\sim Ueq, Uanis(C9S') \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O3S') = Uanis(O3S)
6. Others
 Sof(O2S')=Sof(N2S')=Sof(C4S')=Sof(H4S')=Sof(C5S')=Sof(H5SD)=Sof(H5SE)=
 Sof(H5SF)=Sof(C6S')=Sof(H6SD)=Sof(H6SE)=Sof(H6SF)=1-FVAR(1)
 Sof(O2S)=Sof(N2S)=Sof(C4S)=Sof(H4S)=Sof(C5S)=Sof(H5SA)=Sof(H5SB)=Sof(H5SC)=
 Sof(C6S)=Sof(H6SA)=Sof(H6SB)=Sof(H6SC)=FVAR(1)
 Sof(O3S')=Sof(N3S')=Sof(C7S')=Sof(H7S')=Sof(C8S')=Sof(H8SD)=Sof(H8SE)=
 Sof(H8SF)=Sof(C9S')=Sof(H9SD)=Sof(H9SE)=Sof(H9SF)=1-FVAR(2)
 Sof(O3S)=Sof(N3S)=Sof(C7S)=Sof(H7S)=Sof(C8S)=Sof(H8SA)=Sof(H8SB)=Sof(H8SC)=
 Sof(C9S)=Sof(H9SA)=Sof(H9SB)=Sof(H9SC)=FVAR(2)
7.a Aromatic/amide H refined with riding coordinates:
 C112(H112), C113(H113), C114(H114), C115(H115), C116(H116), C122(H122),
 C123(H123), C124(H124), C125(H125), C126(H126), C132(H132), C133(H133),
 C134(H134), C135(H135), C136(H136), C212(H212), C213(H213), C214(H214),
 C215(H215), C216(H216), C222(H222), C223(H223), C224(H224), C225(H225),
 C226(H226), C232(H232), C233(H233), C234(H234), C235(H235), C236(H236),
 C312(H312), C313(H313), C314(H314), C315(H315), C316(H316), C322(H322),
 C323(H323), C324(H324), C325(H325), C326(H326), C332(H332), C333(H333),
 C334(H334), C335(H335), C336(H336), C1S(H1S), C4S(H4S), C4S'(H4S'), C7S(H7S),
 C7S'(H7S')
7.b Idealised Me refined as rotating group:
 C2S(H2SA,H2SB,H2SC), C3S(H3SA,H3SB,H3SC), C5S(H5SA,H5SB,H5SC), C6S(H6SA,H6SB,
 H6SC), C5S'(H5SD,H5SE,H5SF), C6S'(H6SD,H6SE,H6SF), C8S(H8SA,H8SB,H8SC),
 C9S(H9SA,H9SB,H9SC), C8S'(H8SD,H8SE,H8SF), C9S'(H9SD,H9SE,H9SF)
;
_shelx_res_checksum              31882
_olex2_submission_special_instructions 'No special instructions were received'