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_1557223
_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, C H2 Cl2, 0.9[C4H10O1]'
_chemical_formula_sum            'C55.6 H49 Br2 Cl2 Cu F6 N2 O1.9 P3'
_chemical_formula_weight         1276.74
_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             2019-10-07
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                70.366(3)
_cell_angle_beta                 86.491(3)
_cell_angle_gamma                73.206(3)
_cell_formula_units_Z            2
_cell_length_a                   10.9300(4)
_cell_length_b                   14.2927(6)
_cell_length_c                   19.2894(8)
_cell_measurement_reflns_used    63311
_cell_measurement_temperature    130
_cell_measurement_theta_max      57.39
_cell_measurement_theta_min      2.98
_cell_volume                     2715.0(2)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.153.0 (STOE, 2018)
;
_computing_data_reduction
;
X-Area Integrate 1.74.2.0 (STOE, 2018)
X-Area LANA 1.75.3.0 (STOE, 2018)
;
_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_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  Basel-Ga-Metaljet
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '1.2 0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34143
_diffrn_reflns_av_R_equivalents  0.0795
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            32020
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        53.597
_diffrn_reflns_theta_max         57.052
_diffrn_reflns_theta_min         2.980
_diffrn_source                   'Metaljet D2'
_diffrn_source_current           3.570
_diffrn_source_power             0.250
_diffrn_source_voltage           70
_exptl_absorpt_coefficient_mu    4.864
_exptl_absorpt_correction_T_max  0.7935
_exptl_absorpt_correction_T_min  0.0021
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_description       block
_exptl_crystal_F_000             1288
_exptl_crystal_recrystallization_method
;
The material was recrystallised from a mixture of DCM and Et2O
by solvent layering
;
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.114
_refine_diff_density_min         -1.541
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     624
_refine_ls_number_reflns         10645
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_gt           0.0858
_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^)+(0.1429P)^2^+6.6493P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2317
_refine_ls_wR_factor_ref         0.2384
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9958
_reflns_number_total             10645
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ISN165_130K.cif
_cod_data_source_block           isn165_130k
_cod_original_formula_sum        'C55.60 H49 Br2 Cl2 Cu F6 N2 O1.90 P3'
_cod_database_code               1557223
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.529
_shelx_estimated_absorpt_t_min   0.529
_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.a Secondary CH2 refined with riding coordinates:
 C52(H52A,H52B)
2.b Aromatic/amide H refined with riding coordinates:
 C43(H43), C42(H42), C35(H35), C2(H2), C44(H44), C10(H10), C12(H12), C30(H30),
 C36(H36), C41(H41), C45(H45), C20(H20), C28(H28), C29(H29), C47(H47), C37(H37),
  C11(H11), C49(H49), C14(H14), C21(H21), C51(H51), C1(H1), C48(H48), C24(H24),
 C9(H9), C18(H18), C50(H50), C23(H23), C15(H15), C22(H22), C16(H16), C17(H17)
2.c Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C38(H38A,H38B,H38C)
;
_shelx_res_checksum              13159
_shelx_hkl_checksum              54484
_shelx_fab_checksum              95260
_olex2_date_sample_data_collection 2019-09-07
_olex2_date_sample_submission    2019-05-27
_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 ISN165_130K
_olex2_submission_special_instructions 'No special instructions were received'