Heteroleptic [Cu(P^P)(N^N)][PF6] Compounds with Isomeric Dibromo-1,10-Phenanthroline Ligands
Nohara, Isaak; Keller, Aramis; Tarassenko, Nikolai; Prescimone, Alessandro; Constable, Edwin C.; Housecroft, Catherine E.; Inorganics 8 (2020) 4–; doi:10.3390/inorganics8010004

data_1557226
_publ_section_title
;
 Heteroleptic [Cu(P^P)(N^N)][PF6] Compounds with Isomeric
 Dibromo-1,10-Phenanthroline Ligands
;
_journal_issue                   1
_journal_name_full               Inorganics
_journal_page_first              4
_journal_paper_doi               10.3390/inorganics8010004
_journal_volume                  8
_journal_year                    2020
_chemical_formula_moiety
'C51 H38 Br2 Cu N2 O P2, F6 P, 1.1(C H2 Cl2), 0.7(C4 H10 O)'
_chemical_formula_sum            'C54.9 H47.2 Br2 Cl2.2 Cu F6 N2 O1.7 P3'
_chemical_formula_weight         1270.40
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-05
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90.204(2)
_cell_angle_beta                 98.120(2)
_cell_angle_gamma                99.535(2)
_cell_formula_units_Z            2
_cell_length_a                   10.1768(8)
_cell_length_b                   13.7504(11)
_cell_length_c                   20.1505(16)
_cell_measurement_reflns_used    9933
_cell_measurement_temperature    130
_cell_measurement_theta_max      70.216
_cell_measurement_theta_min      3.892
_cell_volume                     2751.9(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      130
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            35742
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.285
_diffrn_reflns_theta_min         3.260
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.597
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.6260
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0565 before and 0.0342 after correction.
The Ratio of minimum to maximum transmission is 0.8310.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_description       block
_exptl_crystal_F_000             1279
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of Et2O and DCM  by solvent layering'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.497
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     728
_refine_ls_number_reflns         10241
_refine_ls_number_restraints     136
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0592P)^2^+3.7381P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1093
_refine_ls_wR_factor_ref         0.1101
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9939
_reflns_number_total             10241
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ISN162_130K_0m.cif
_cod_data_source_block           isn162_130k_0m
_cod_original_formula_sum        'C54.90 H47.20 Br2 Cl2.20 Cu F6 N2 O1.70 P3'
_cod_database_code               1557226
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.632
_shelx_estimated_absorpt_t_min   0.492
_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
 O2-C54 = O2-C55
 1.45 with sigma of 0.02
 C53-C54 = C56-C55
 1.5 with sigma of 0.02
 O2-C55 \\sim O2-C54
 with sigma of 0.02
 C53-C54 \\sim C55-C56
 with sigma of 0.02
 Cl3-C57 \\sim Cl4-C57 \\sim Cl2_$1-C52_$1 \\sim Cl1_$1-C52_$1 \\sim C58-Cl7
\\sim C58-Cl8 \\sim C59-
 Cl6 \\sim C59-Cl5
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Cl2) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(Cl1) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C53) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(C55)
\\sim Ueq, Uanis(C56) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(Cl3) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(Cl4) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(Cl6) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(Cl5) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(Cl7) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(Cl8) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(Cl3) = Uanis(C57) = Uanis(Cl4)
Uanis(Cl7) = Uanis(C58) = Uanis(Cl8)
4. Others
 Fixed Sof: Cl2(0.5) Cl1(0.5) C52(0.5) H52A(0.5) H52B(0.5) O2(0.7) C55(0.7)
 H55A(0.7) H55B(0.7) C54(0.7) H54A(0.7) H54B(0.7) C56(0.7) H56A(0.7) H56B(0.7)
 H56C(0.7) C53(0.7) H53A(0.7) H53B(0.7) H53C(0.7) Cl4(0.3) Cl3(0.3) C57(0.3)
 H57A(0.3) H57B(0.3) Cl6(0.2) Cl7(0.1) Cl8(0.1) Cl5(0.2) C58(0.1) H58A(0.1)
 H58B(0.1) C59(0.2) H59A(0.2) H59B(0.2)
5.a Secondary CH2 refined with riding coordinates:
 C52(H52A,H52B), C55(H55A,H55B), C54(H54A,H54B), C57(H57A,H57B), C58(H58A,
 H58B), C59(H59A,H59B)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C39(H39), C20(H20), C47(H47), C38(H38), C37(H37), C3(H3), C41(H41),
 C23(H23), C22(H22), C24(H24), C48(H48), C32(H32), C12(H12), C14(H14), C10(H10),
  C18(H18), C45(H45), C21(H21), C8(H8), C33(H33), C42(H42), C9(H9), C43(H43),
 C34(H34), C44(H44), C15(H15), C51(H51), C49(H49), C16(H16), C17(H17), C50(H50)
5.c Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C35(H35A,H35B,H35C), C56(H56A,H56B,H56C), C53(H53A,H53B,
 H53C)
;
_shelx_res_checksum              67339
_shelx_hkl_checksum              30322
_olex2_date_sample_data_collection 2019-06-02
_olex2_date_sample_submission    2019-05-25
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a mylar loop in perfluoroether oil'
_olex2_submission_original_sample_id ISN162_130K
_olex2_submission_special_instructions 'No special instructions were received'