Studies Relevant to the Functional Model of Mo-Cu CODH: In Situ Reactions of Cu(I)-L Complexes with Mo(VI) and Synthesis of Stable Structurally Characterized Heterotetranuclear Mo<sup>VI</sup><sub>2</sub>Cu<sup>I</sup><sub>2</sub> Complex.
Kaluarachchige Don, Umesh I.; Almaat, Ahmad S.; Ward, Cassandra L.; Groysman, Stanislav; Molecules (Basel, Switzerland) 28 (2023) 3644–; doi:10.3390/molecules28083644

data_1569073
_publ_section_title
;
 Studies Relevant to the Functional Model of Mo-Cu CODH: In Situ Reactions
 of Cu(I)-L Complexes with Mo(VI) and Synthesis of Stable Structurally
 Characterized Heterotetranuclear
 Mo<sup>VI</sup><sub>2</sub>Cu<sup>I</sup><sub>2</sub> Complex.
;
_journal_issue                   8
_journal_name_full               'Molecules (Basel, Switzerland)'
_journal_page_first              3644
_journal_paper_doi               10.3390/molecules28083644
_journal_volume                  28
_journal_year                    2023
_chemical_formula_moiety
'C84 H88 Cu2 Mo2 N8 O11, C18 H16 O Si, 6(C2 H3 N)'
_chemical_formula_sum            'C114 H122 Cu2 Mo2 N14 O12 Si'
_chemical_formula_weight         2227.30
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2023-03-13
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_cell_angle_alpha                90
_cell_angle_beta                 109.253(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.546(5)
_cell_length_b                   21.591(7)
_cell_length_c                   25.679(7)
_cell_measurement_reflns_used    22266
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.50
_cell_measurement_theta_min      1.91
_cell_volume                     10754(5)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-1997  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Photon III'
_diffrn_detector_type            'CPAD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       '\k--geometry diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_collimation    '0.8 mm pinhole collimator'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1084
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            386980
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.980
_diffrn_reflns_theta_min         1.911
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Incoatec I\mS'
_exptl_absorpt_coefficient_mu    0.696
_exptl_absorpt_correction_T_max  0.9660
_exptl_absorpt_correction_T_min  0.9027
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.'
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4624
_exptl_crystal_recrystallization_method 'acetonitrile ether benzene'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.809
_refine_diff_density_min         -1.303
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1369
_refine_ls_number_reflns         25749
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0996
_refine_ls_R_factor_gt           0.0682
_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^)+(0.0794P)^2^+46.7579P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1760
_refine_ls_wR_factor_ref         0.1977
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18373
_reflns_number_total             25749
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            sg982_final_CLW.cif
_cod_data_source_block           sg982_final
_cod_database_code               1569073
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.903
_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, All O(H) groups
2. Uiso/Uaniso restraints and constraints
C61 \\sim C1B \\sim C2A \\sim C3B \\sim C4A \\sim C3A \\sim C4B \\sim C2B \\sim
C1A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
3. Others
 Sof(C1B)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=Sof(H2BC)=Sof(C3B)=Sof(H3BA)=Sof(H3BB)=
 Sof(H3BC)=Sof(C4B)=Sof(H4BA)=Sof(H4BB)=Sof(H4BC)=1-FVAR(1)
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C2A)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=
 Sof(H3AC)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C19(H19A,H19B), C52(H52A,H52B), C53(H53A,H53B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C14(H14),
 C15(H15), C16(H16), C17(H17), C21(H21), C23(H23), C31(H31), C33(H33), C41(H41),
  C42(H42), C43(H43), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50),
 C55(H55), C56(H56), C57(H57), C58(H58), C60(H60), C62(H62), C73(H73), C75(H75),
  C79(H79), C80(H80), C81(H81), C82(H82), C83(H83), C84(H84), C85(H85),
 C86(H86), C87(H87), C88(H88), C89(H89), C90(H90), C91(H91), C92(H92), C93(H93)
4.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C34(H34A,H34B,H34C), C35(H35A,H35B,
 H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,
 H39B,H39C), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C), C76(H76A,H76B,H76C),
 C77(H77A,H77B,H77C), C78(H78A,H78B,H78C), C1A(H1AA,H1AB,H1AC), C3A(H3AA,H3AB,
 H3AC), C4A(H4AA,H4AB,H4AC), C2B(H2BA,H2BB,H2BC), C3B(H3BA,H3BB,H3BC), C4B(H4BA,
 H4BB,H4BC), C99(H99A,H99B,H99C), C95(H95A,H95B,H95C), C97(H97A,H97B,H97C),
 C94(H94A,H94B,H94C), C96(H96A,H96B,H96C), C98(H98A,H98B,H98C)
4.d Idealised tetrahedral OH refined as rotating group:
 O12(H12)
;
_shelx_res_checksum              97471
_shelx_hkl_checksum              89320
_olex2_submission_special_instructions 'No special instructions were received'