Incorporation of coinage metal-NHC complexes into heptaphosphide clusters.
Jo, Minyoung; Li, Jingbai; Dragulescu-Andrasi, Alina; Rogachev, Andrey Yu; Shatruk, Michael; Dalton transactions (Cambridge, England : 2003) 49 (2020) 12955–12959; doi:10.1039/d0dt03119d

data_7705403
_publ_section_title
;
 Incorporation of coinage metal-NHC complexes into heptaphosphide
 clusters.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12955
_journal_page_last               12959
_journal_paper_doi               10.1039/d0dt03119d
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C54 H72 Cu N4, C30 H45 Cu N2 P7 Si'
_chemical_formula_sum            'C84 H117 Cu2 N6 P7 Si'
_chemical_formula_weight         1582.79
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-01-15
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2018.12.05 svn.r3537 for Rigaku Oxford Diffraction, GUI svn.r5625)
;
_audit_update_record
;
2020-01-18 deposited with the CCDC.	2020-09-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.290(2)
_cell_length_b                   25.025(2)
_cell_length_c                   28.319(3)
_cell_measurement_reflns_used    9888
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      19.19
_cell_measurement_theta_min      2.21
_cell_volume                     17214(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1058
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            158052
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.713
_diffrn_reflns_theta_max         24.713
_diffrn_reflns_theta_min         1.168
_exptl_absorpt_coefficient_mu    0.683
_exptl_absorpt_correction_T_max  0.7443
_exptl_absorpt_correction_T_min  0.7007
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/2 (Bruker, 2014)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_description       block
_exptl_crystal_F_000             6720
_exptl_crystal_recrystallization_method 'Slow evaporation of THF solution'
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.848
_refine_diff_density_min         -1.920
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     956
_refine_ls_number_reflns         14686
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1389
_refine_ls_R_factor_gt           0.0882
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0930P)^2^+81.4089P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2103
_refine_ls_wR_factor_ref         0.2456
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9365
_reflns_number_total             14686
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03119d2.cif
_cod_data_source_block           Cu-NHC-P7
_cod_depositor_comments
'Adding full bibliography for 7705403--7705404.cif.'
_cod_database_code               7705403
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.821
_shelx_estimated_absorpt_t_min   0.726
_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. Uiso/Uaniso restraints and constraints
Uanis(P7A) = Uanis(P7B)
Uanis(P2A) = Uanis(P5B)
Uanis(P5A) = Uanis(P2B)
Uanis(P3A) = Uanis(P4B)
Uanis(P4A) = Uanis(P3B)
Uanis(P6A) = Uanis(P6B)
3. Others
 Sof(P5B)=Sof(P2B)=Sof(P4B)=Sof(P6B)=Sof(P3B)=Sof(P7B)=Sof(P1B)=1-FVAR(1)
 Sof(P4A)=Sof(P2A)=Sof(P5A)=Sof(P7A)=Sof(P3A)=Sof(P6A)=Sof(P1A)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C21(H21), C68(H68), C75(H75), C41(H41), C34(H34), C48(H48), C7(H7), C82(H82),
 C61(H61), C55(H55), C28(H28), C14(H14)
4.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C17(H17), C37(H37), C44(H44), C39(H39), C64(H64), C45(H45),
 C66(H66), C38(H38), C78(H78), C51(H51), C65(H65), C80(H80), C79(H79), C53(H53),
  C24(H24), C52(H52), C71(H71), C72(H72), C11(H11), C10(H10), C26(H26),
 C25(H25), C12(H12)
4.c Idealised Me refined as rotating group:
 C62(H62A,H62B,H62C), C35(H35A,H35B,H35C), C22(H22A,H22B,H22C), C50(H50A,H50B,
 H50C), C49(H49A,H49B,H49C), C70(H70A,H70B,H70C), C69(H69A,H69B,H69C), C23(H23A,
 H23B,H23C), C57(H57A,H57B,H57C), C16(H16A,H16B,H16C), C2(H2A,H2B,H2C),
 C43(H43A,H43B,H43C), C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C36(H36A,H36B,H36C),
 C84(H84A,H84B,H84C), C9(H9A,H9B,H9C), C42(H42A,H42B,H42C), C63(H63A,H63B,H63C),
  C76(H76A,H76B,H76C), C77(H77A,H77B,H77C), C56(H56A,H56B,H56C), C29(H29A,H29B,
 H29C), C8(H8A,H8B,H8C), C83(H83A,H83B,H83C), C15(H15A,H15B,H15C), C30(H30A,
 H30B,H30C)
;
_shelx_res_checksum              84205
_olex2_submission_special_instructions 'No special instructions were received'