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_1557227
_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
'0.5(C102 H76 Br4 Cu2 N4 O2 P4), F6 P, 1.1[CH2Cl2]'
_chemical_formula_sum            'C52.1 H40.2 Br2 Cl2.2 Cu F6 N2 O P3'
_chemical_formula_weight         1218.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-08-16
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.059(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   33.3182(16)
_cell_length_b                   14.1050(6)
_cell_length_c                   11.8205(5)
_cell_measurement_reflns_used    30478
_cell_measurement_temperature    130
_cell_measurement_theta_max      57.32
_cell_measurement_theta_min      3.33
_cell_volume                     5432.5(4)
_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 0.991
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details      ' 2284 frames, detector distance = 60 mm'
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'Stoe StadiVari'
_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  0.0515
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15005
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        53.597
_diffrn_reflns_theta_max         56.714
_diffrn_reflns_theta_min         3.326
_diffrn_source                   'Metaljet D2'
_diffrn_source_current           3.570
_diffrn_source_power             0.250
_diffrn_source_voltage           70
_exptl_absorpt_coefficient_mu    4.895
_exptl_absorpt_correction_T_max  0.9092
_exptl_absorpt_correction_T_min  0.0046
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
Afterwards scaling of reflection intensities was performed within STOE LANA.
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.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_description       plate
_exptl_crystal_F_000             2441
_exptl_crystal_recrystallization_method
;
The material was recrystallised from a mixture of DCM and Et2O 
by solvent layering
;
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.163
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.117
_refine_diff_density_min         -0.791
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         5607
_refine_ls_number_restraints     156
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0863
_refine_ls_R_factor_gt           0.0728
_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^)+(0.0865P)^2^+41.9785P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1853
_refine_ls_wR_factor_ref         0.1973
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4802
_reflns_number_total             5607
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ISN166_130K.cif
_cod_data_source_block           isn166_130k
_cod_original_formula_sum        'C52.10 H40.20 Br2 Cl2.20 Cu F6 N2 O P3'
_cod_database_code               1557227
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.828
_shelx_estimated_absorpt_t_min   0.374
_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. Restrained distances
 C23-C21 \\sim C24-C23 \\sim C24-C25 \\sim C26-C25 \\sim C27-C26 \\sim C27-C21
 with sigma of 0.02
 C37-C13 \\sim C33-C13 \\sim C33-C34 \\sim C35-C34 \\sim C35-C36 \\sim C36-C37
 with sigma of 0.02
 C8-C7 \\sim C12-C7 \\sim C11-C12 \\sim C9-C8
 with sigma of 0.02
3. Restrained planarity
 C13, C33, C34, C35, C36, C37
 with sigma of 0.1
 C21, C27, C26, C25, C24, C23
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C20) \\sim Ueq, Uanis(C23) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C21) = Uanis(C20) = Uanis(C19) = Uanis(C18) = Uanis(C17) = Uanis(C22)
5. Rigid body (RIGU) restrains
 C21, C27, C26, C25, C24, C23
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C13, C33, C34, C35, C36, C37
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C7, C8, C9, C12, C11, C10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C20(0.5) H20(0.5) C19(0.5) H19(0.5) O1(0.5) C18(0.5) H18(0.5)
 C15(0.5) C22(0.5) C14(0.5) C17(0.5) C29(0.5) H29A(0.5) H29B(0.5) H29C(0.5)
 C31(0.5) H31(0.5) C28(0.5) H28A(0.5) H28B(0.5) H28C(0.5) C32(0.5) H32(0.5)
 C8(0.5) H8(0.5) C16(0.5) C9(0.5) H9(0.5) C36(0.5) H36(0.5) C12(0.5) H12(0.5)
 C33(0.5) C37(0.5) H37(0.5) C34(0.5) H34(0.5) C35(0.5) H35(0.5) C30(0.5)
 H30(0.5) C11(0.5) H11(0.5) C27(0.5) H27(0.5) C26(0.5) H26(0.5) C25(0.5)
 H25(0.5) C24(0.5) H24(0.5) C23(0.5) H23(0.5)
7.a Riding coordinates:
 C31(H31), C32(H32), C8(H8), C9(H9), C33(H33), C10(H10)
7.b Aromatic/amide H refined with riding coordinates:
 C39(H39), C20(H20), C40(H40), C43(H43), C41(H41), C42(H42), C2(H2), C19(H19),
 C3(H3), C6(H6), C18(H18), C36(H36), C12(H12), C37(H37), C34(H34), C35(H35),
 C30(H30), C11(H11), C27(H27), C26(H26), C25(H25), C24(H24), C23(H23)
7.c Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              55952
_shelx_hkl_checksum              79017
_shelx_fab_checksum              29157
_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 ISN166_130K
_olex2_submission_special_instructions 'No special instructions were received'