Crystal structure of 1,1′-bis(diphenylphosphino)ferrocene-(1,1′-bis(diphenylphosphino)ferrocene-κ2 P,P′)-(O-isobutyl sulfurodithioito-κ2 S,S′)copper(I), C39H37CuFeOP2S2
Li, Zhuang-yu; Liu, Xiao-jing; Liu, E.; Jian, Fang-fang; Liang, Tongling; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 935–937; doi:10.1515/ncrs-2020-0108

data_8105336
_publ_section_title
;
 Crystal structure of
 1,1&#x2032;-bis(diphenylphosphino)ferrocene-(1,1&#x2032;-bis(diphenylphosphino)ferrocene-\k2
 P,P&#x2032;)-(O-isobutyl sulfurodithioito-\k2 S,S&#x2032;)copper(I),
 C39H37CuFeOP2S2
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              935
_journal_page_last               937
_journal_paper_doi               10.1515/ncrs-2020-0108
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C39 H37 Cu Fe O P2 S2'
_chemical_formula_sum            'C39 H37 Cu Fe O P2 S2'
_chemical_formula_weight         767.20
_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
_atom_sites_solution_primary     direct
_cell_angle_alpha                99.732(2)
_cell_angle_beta                 96.342(2)
_cell_angle_gamma                93.446(2)
_cell_formula_units_Z            2
_cell_length_a                   9.6132(10)
_cell_length_b                   11.5667(12)
_cell_length_c                   16.8739(18)
_cell_measurement_reflns_used    3634
_cell_measurement_temperature    293
_cell_measurement_theta_max      26.110
_cell_measurement_theta_min      2.334
_cell_volume                     1832.0(3)
_computing_cell_refinement       'SAINT v7.23A (Bruker, 2003)'
_computing_data_reduction        'SAINT v7.23A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.9890
_diffrn_measured_fraction_theta_max 0.9890
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4 diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0174
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12016
_diffrn_reflns_theta_full        25.4986
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    1.207
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'clear brownish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.3907
_exptl_crystal_description       block
_exptl_crystal_F_000             794.5064
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.6773
_refine_diff_density_min         -0.4924
_refine_diff_density_rms         0.0832
_refine_ls_d_res_high            0.8255
_refine_ls_d_res_low             11.3633
_refine_ls_goodness_of_fit_ref   1.0521
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    79
_refine_ls_number_parameters     442
_refine_ls_number_reflns         6745
_refine_ls_number_restraints     352
_refine_ls_restrained_S_all      1.0239
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0455
_refine_ls_shift/su_max          0.0004
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0516P)^2^+1.9148P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1212
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              13
_reflns_limit_k_min              -14
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                5281
_reflns_number_total             6745
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            suppl_ncrs-2020-0108_suppl.cif
_cod_data_source_block           QJ07134
_cod_database_code               8105336
_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
2. Restrained distances
 C37A-C36A = C37B-C36B = C39-C37A = C39-C37B = C38A-C37A = C38B-C37B
 1.54 with sigma of 0.01
 O1-C36B = O1-C36A
 1.47 with sigma of 0.01
 C36B-C38B
 2.5 with sigma of 0.02
3. Rigid bond restraints
 S2, C35
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C36A \\sim C37A \\sim C38A \\sim C36B \\sim C37B \\sim C38B \\sim C39 \\sim O1:
within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C36A \\sim C37A \\sim C38A \\sim C36B \\sim C37B
\\sim C38B \\sim C39: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01
C35 \\sim S1 \\sim S2 \\sim O1: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C36A) \\sim Ueq, Uanis(C37A) \\sim Ueq, Uanis(C38A) \\sim Ueq,
Uanis(C36B) \\sim Ueq, Uanis(C37B) \\sim Ueq, Uanis(C38B) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(C37A)=Sof(H37A)=Sof(C36B)=Sof(H36c)=Sof(H36d)=Sof(C38B)=Sof(H38d)=
 Sof(H38e)=Sof(H38f)=1-FVAR(1)
 Sof(C36A)=Sof(H36a)=Sof(H36b)=Sof(C38A)=Sof(H38a)=Sof(H38b)=Sof(H38c)=
 Sof(C37B)=Sof(H37B)=FVAR(1)
6.a Riding coordinates:
 C39(H39a,H39b,H39c)
6.b Ternary CH refined with riding coordinates:
 C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32),
 C33(H33), C37A(H37A), C37B(H37B)
6.c Secondary CH2 refined with riding coordinates:
 C36A(H36a,H36b), C36B(H36c,H36d)
6.d Me refined with riding coordinates:
 C38A(H38a,H38b,H38c), C38B(H38d,H38e,H38f)
6.e Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10),
 C11(H11), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20),
  C21(H21), C22(H22), C23(H23)
;
_olex2_submission_special_instructions 'No special instructions were received'