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_1569072
_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         'C51 H55 Cu N5 O3, F6 P, C4 H10 O'
_chemical_formula_sum            'C55 H65 Cu F6 N5 O4 P'
_chemical_formula_weight         1068.670
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_audit_creation_date             2023-01-19
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_cell_angle_alpha                112.847(1)
_cell_angle_beta                 92.606(1)
_cell_angle_gamma                109.383(1)
_cell_formula_units_Z            2
_cell_length_a                   13.6310(5)
_cell_length_b                   14.4630(6)
_cell_length_c                   15.8288(6)
_cell_measurement_reflns_used    10752
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.36
_cell_volume                     2657.65(18)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.9960
_diffrn_measured_fraction_theta_max 0.9968
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_Laue_measured_fraction_full 0.9960
_diffrn_reflns_Laue_measured_fraction_max 0.9968
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            136640
_diffrn_reflns_point_group_measured_fraction_full 0.9960
_diffrn_reflns_point_group_measured_fraction_max 0.9968
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.36
_exptl_absorpt_coefficient_mu    0.512
_exptl_absorpt_correction_T_max  0.9651
_exptl_absorpt_correction_T_min  0.9272
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_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    1.335
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1121.700
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.4999
_refine_diff_density_min         -0.3728
_refine_diff_density_rms         0.0635
_refine_ls_d_res_high            0.7696
_refine_ls_d_res_low             8.6303
_refine_ls_goodness_of_fit_ref   1.0400
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    99
_refine_ls_number_parameters     668
_refine_ls_number_reflns         12161
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0400
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          -0.0004
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0511P)^2^+1.7867P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.1011
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              16
_reflns_limit_k_min              -18
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                10752
_reflns_number_total             12161
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            sg988_0m.cif
_cod_data_source_block           sg988_0m
_cod_database_code               1569072
_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.a Secondary CH2 refined with riding coordinates:
 C53(H53a,H53b), C15(H15a,H15b), C50(H50a,H50b), C51(H51a,H51b)
2.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C19(H19), C18(H18), C17(H17), C42(H42), C46(H46), C45(H45),
 C44(H44), C35(H35), C37(H37), C24(H24), C22(H22), C13(H13), C12(H12), C56(H56),
  C10(H10), C7(H7), C54(H54), C5(H5)
2.c Idealised Me refined as rotating group:
 C55(H55a,H55b,H55c), C39(H39a,H39b,H39c), C40(H40a,H40b,H40c), C41(H41a,H41b,
 H41c), C57(H57a,H57b,H57c), C30(H30a,H30b,H30c), C58(H58a,H58b,H58c), C31(H31a,
 H31b,H31c), C4(H4a,H4b,H4c), C9(H9a,H9b,H9c), C49(H49a,H49b,H49c), C52(H52a,
 H52b,H52c)
;
_olex2_submission_special_instructions 'No special instructions were received'