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_7249039
_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 H94 Ag4 Mo8 N2 O26 P8, 2(C H2 Cl2), 2(C2 H3 N)'
_chemical_formula_sum            'C110 H104 Ag4 Cl4 Mo8 N4 O26 P8'
_chemical_formula_weight         3486.53
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-06-26
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.7515(8)
_cell_length_b                   17.9116(6)
_cell_length_c                   33.5518(11)
_cell_measurement_reflns_used    9925
_cell_measurement_temperature    200.00
_cell_measurement_theta_max      56.123
_cell_measurement_theta_min      3.434
_cell_volume                     14273.9(8)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      200.00
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0628
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            136260
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         57.325
_diffrn_reflns_theta_min         3.238
_exptl_absorpt_coefficient_mu    7.975
_exptl_absorpt_correction_T_max  0.285
_exptl_absorpt_correction_T_min  0.185
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'blessing, Acta Cryst. 1995(A51) 33-38'
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_description       block
_exptl_crystal_F_000             6848
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.599
_refine_diff_density_min         -0.963
_refine_diff_density_rms         0.170
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.498(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1290
_refine_ls_number_reflns         26085
_refine_ls_number_restraints     500
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0539
_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^)+(0.0821P)^2^+60.0424P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1373
_refine_ls_wR_factor_ref         0.1396
_reflns_Friedel_coverage         0.966
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.968
_reflns_number_gt                24205
_reflns_number_total             26085
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00496e2.cif
_cod_data_source_block           w_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7249036--7249039.cif.'
_cod_database_code               7249039
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.285
_shelx_estimated_absorpt_t_min   0.185
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.502(12)
 0.498(12)
2. 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
3. Restrained distances
 C1S-Cl1S = C1S-Cl2S
 1.78 with sigma of 0.01
 C2S-Cl3S = C2S-Cl4S
 1.78 with sigma of 0.01
 C11-C12 = C13-C14 = C3S-C4S = C5S-C6S
 1.45 with sigma of 0.01
4. Rigid bond restraints
 C11, C12, C13, C14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1S, Cl1S, Cl2S
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C2S, Cl3S, Cl4S
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1, P1, C1, P2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C111, C112, C113, C114, C115, C116
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C621, C622, C623, C624, C625, C626
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C11 \\sim C12 \\sim C13 \\sim C14: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C1S \\sim Cl1S \\sim Cl2S: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C2S \\sim Cl3S \\sim Cl4S: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C1 \\sim P1 \\sim P2: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 2A
C111 \\sim C112 \\sim C113 \\sim C114 \\sim C115 \\sim C116: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C621 \\sim C622 \\sim C623 \\sim C624 \\sim C625 \\sim C626: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14)
\\sim Ueq, Uanis(C123) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C1S) \\sim Ueq, Uanis(Cl1S) \\sim Ueq, Uanis(Cl2S) \\sim Ueq, Uanis(C1)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C2S) \\sim Ueq, Uanis(Cl3S) \\sim Ueq, Uanis(Cl4S) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O19) \\sim Ueq, Uanis(O20)
\\sim Ueq, Uanis(O16) \\sim Ueq, Uanis(C812) \\sim Ueq, Uanis(C311) \\sim Ueq:
with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C211) \\sim Ueq, Uanis(C715) \\sim Ueq, Uanis(C725) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C111) \\sim Ueq, Uanis(C112) \\sim Ueq, Uanis(C113) \\sim Ueq,
Uanis(C114) \\sim Ueq, Uanis(C115) \\sim Ueq, Uanis(C116) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C311) \\sim Ueq, Uanis(C312) \\sim Ueq, Uanis(C313) \\sim Ueq,
Uanis(C314) \\sim Ueq, Uanis(C315) \\sim Ueq, Uanis(C316) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C321) \\sim Ueq, Uanis(C322) \\sim Ueq, Uanis(C323) \\sim Ueq,
Uanis(C324) \\sim Ueq, Uanis(C325) \\sim Ueq, Uanis(C326) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C411) \\sim Ueq, Uanis(C412) \\sim Ueq, Uanis(C413) \\sim Ueq,
Uanis(C414) \\sim Ueq, Uanis(C415) \\sim Ueq, Uanis(C416) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C511) \\sim Ueq, Uanis(C512) \\sim Ueq, Uanis(C513) \\sim Ueq,
Uanis(C514) \\sim Ueq, Uanis(C515) \\sim Ueq, Uanis(C516) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C621) \\sim Ueq, Uanis(C622) \\sim Ueq, Uanis(C623) \\sim Ueq,
Uanis(C624) \\sim Ueq, Uanis(C625) \\sim Ueq, Uanis(C626) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C1S(H1SA,H1SB), C2S(H2SA,
 H2SB)
6.b 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), C212(H212), C213(H213),
 C214(H214), C215(H215), C216(H216), C222(H222), C223(H223), C224(H224),
 C225(H225), C226(H226), C312(H312), C313(H313), C314(H314), C315(H315),
 C316(H316), C322(H322), C323(H323), C324(H324), C325(H325), C326(H326),
 C412(H412), C413(H413), C414(H414), C415(H415), C416(H416), C422(H422),
 C423(H423), C424(H424), C425(H425), C426(H426), C512(H512), C513(H513),
 C514(H514), C515(H515), C516(H516), C522(H522), C523(H523), C524(H524),
 C525(H525), C526(H526), C612(H612), C613(H613), C614(H614), C615(H615),
 C616(H616), C622(H622), C623(H623), C624(H624), C625(H625), C626(H626),
 C712(H712), C713(H713), C714(H714), C715(H715), C716(H716), C722(H722),
 C723(H723), C724(H724), C725(H725), C726(H726), C812(H812), C813(H813),
 C814(H814), C815(H815), C816(H816), C822(H822), C823(H823), C824(H824),
 C825(H825), C826(H826)
6.c Fitted hexagon refined as free rotating group:
 C111(C112,C113,C114,C115,C116), C121(C122,C123,C124,C125,C126), C211(C212,
 C213,C214,C215,C216), C221(C222,C223,C224,C225,C226), C311(C312,C313,C314,C315,
 C316), C321(C322,C323,C324,C325,C326), C411(C412,C413,C414,C415,C416),
 C421(C422,C423,C424,C425,C426), C511(C512,C513,C514,C515,C516), C521(C522,C523,
 C524,C525,C526), C611(C612,C613,C614,C615,C616), C621(C622,C623,C624,C625,
 C626), C711(C712,C713,C714,C715,C716), C721(C722,C723,C724,C725,C726),
 C811(C812,C813,C814,C815,C816), C821(C822,C823,C824,C825,C826)
6.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C4S(H4SA,H4SB,H4SC), C6S(H6SA,H6SB,
 H6SC)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              78492
_shelx_fab_checksum              25738
_olex2_submission_special_instructions 'No special instructions were received'