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_1557225
_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         'C48 H34 Br2 Cu N2 O P2, F6 P, 0.5(C4 H10 O)'
_chemical_formula_sum            'C50 H39 Br2 Cu F6 N2 O1.5 P3'
_chemical_formula_weight         1122.10
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-08-15
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                107.867(2)
_cell_angle_beta                 104.444(2)
_cell_angle_gamma                101.088(2)
_cell_formula_units_Z            4
_cell_length_a                   15.1949(10)
_cell_length_b                   18.5322(12)
_cell_length_c                   18.5423(13)
_cell_measurement_reflns_used    9863
_cell_measurement_temperature    130
_cell_measurement_theta_max      70.14
_cell_measurement_theta_min      2.62
_cell_volume                     4603.2(5)
_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 0.974
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \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  0.0241
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            38972
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.266
_diffrn_reflns_theta_min         2.619
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.260
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.5474
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0583 before and 0.0303 after correction.
The Ratio of minimum to maximum transmission is 0.7267.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_description       block
_exptl_crystal_F_000             2252
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of Et2O and DCM  by solvent layering'
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.220
_refine_diff_density_min         -0.823
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1182
_refine_ls_number_reflns         16488
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0369
_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^)+(0.0478P)^2^+6.9335P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0952
_refine_ls_wR_factor_ref         0.0971
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15466
_reflns_number_total             16488
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ISN167_130K_0m.cif
_cod_data_source_block           isn167_130k_0m
_cod_original_formula_sum        'C50 H39 Br2 Cu F6 N2 O1.50 P3'
_cod_database_code               1557225
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.700
_shelx_estimated_absorpt_t_min   0.441
_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 Riding coordinates:
 C99(H99A,H99B), C97(H97A,H97B)
2.b Aromatic/amide H refined with riding coordinates:
 C62(H62), C64(H64), C36(H36), C78(H78), C66(H66), C8(H8), C68(H68), C33(H33),
 C70(H70), C65(H65), C38(H38), C30(H30), C63(H63), C20(H20), C75(H75), C80(H80),
  C9(H9), C40(H40), C44(H44), C69(H69), C2(H2), C81(H81), C83(H83), C72(H72),
 C77(H77), C76(H76), C3(H3), C42(H42), C41(H41), C14(H14), C86(H86), C39(H39),
 C35(H35), C29(H29), C18(H18), C82(H82), C34(H34), C71(H71), C90(H90), C27(H27),
  C50(H50), C11(H11), C51(H51), C57(H57), C48(H48), C15(H15), C46(H46),
 C45(H45), C56(H56), C28(H28), C23(H23), C24(H24), C16(H16), C10(H10), C22(H22),
  C58(H58), C17(H17), C89(H89), C87(H87), C59(H59), C47(H47), C21(H21),
 C88(H88), C92(H92), C94(H94), C96(H96), C93(H93), C95(H95)
2.c Idealised Me refined as rotating group:
 C100(H10A,H10B,H10C), C98(H98A,H98B,H98C)
;
_shelx_res_checksum              8476
_shelx_hkl_checksum              28813
_olex2_date_sample_data_collection 2019-08-14
_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 ISN167_130K
_olex2_submission_special_instructions 'No special instructions were received'