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_7249038
_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
'C72 H60 Cu2 Mo8 O26 P4, 2(C40 H36 Cu N2 P2), 2(C2 H3 N)'
_chemical_formula_sum            'C156 H138 Cu4 Mo8 N6 O26 P8'
_chemical_formula_weight         3782.16
_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             2024-05-15
_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                81.001(2)
_cell_angle_beta                 78.9540(10)
_cell_angle_gamma                88.4190(10)
_cell_formula_units_Z            1
_cell_length_a                   15.9275(6)
_cell_length_b                   16.1794(6)
_cell_length_c                   19.0604(8)
_cell_measurement_reflns_used    9889
_cell_measurement_temperature    200.00
_cell_measurement_theta_max      62.566
_cell_measurement_theta_min      2.928
_cell_volume                     4761.5(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       '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 0.992
_diffrn_measured_fraction_theta_max 0.993
_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  0.0774
_diffrn_reflns_av_unetI/netI     0.0593
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            106468
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         1.820
_diffrn_source_current           3.57
_diffrn_source_power             0.24972149999999999
_diffrn_source_voltage           69.95
_exptl_absorpt_coefficient_mu    1.068
_exptl_absorpt_correction_T_max  0.776
_exptl_absorpt_correction_T_min  0.713
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'blessing, Acta Cryst. 1995(A51) 33-38'
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_description       block
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.759
_refine_diff_density_min         -1.109
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       0.0020(4)
_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   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     941
_refine_ls_number_reflns         19329
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0483
_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^)+(0.0827P)^2^+0.7033P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1467
_refine_ls_wR_factor_ref         0.1563
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13732
_reflns_number_total             19329
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00496e2.cif
_cod_data_source_block           l
_cod_depositor_comments
'Adding full bibliography for 7249036--7249039.cif.'
_cod_database_code               7249038
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.776
_shelx_estimated_absorpt_t_min   0.713
_olex2_refinement_description
;
1. Rigid bond restraints
 C211, C212, C213, C214, C215, C216
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N1S, C1S, C2S
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
2. Uiso/Uaniso restraints and constraints
C211 \\sim C212 \\sim C213 \\sim C214 \\sim C215 \\sim C216: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
N1S \\sim C1S \\sim C2S: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
Uanis(N1S) \\sim Ueq, Uanis(C1S) \\sim Ueq, Uanis(C2S) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
3.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), C412(H412), C413(H413), C414(H414),
 C415(H415), C416(H416), C422(H422), C423(H423), C424(H424), C425(H425),
 C426(H426), C432(H432), C433(H433), C434(H434), C435(H435), C436(H436)
3.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C2S(H2SA,H2SB,H2SC)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              41815
_shelx_fab_checksum              14488
_olex2_submission_special_instructions 'No special instructions were received'