Synthesis and properties of new mononuclear Ru(ii)-based photocatalysts containing 4,4'-diphenyl-2,2'-bipyridyl ligands.
Coe, Benjamin J.; Sánchez, Sergio; Dalton transactions (Cambridge, England : 2003) 45 (2016) 5210–5222; doi:10.1039/c6dt00039h

data_7038378
_publ_section_title
;
 Synthesis and properties of new mononuclear Ru(ii)-based photocatalysts
 containing 4,4'-diphenyl-2,2'-bipyridyl ligands.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5210
_journal_page_last               5222
_journal_paper_doi               10.1039/c6dt00039h
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C25 H36 N O2'
_chemical_formula_sum            'C25 H36 N O2'
_chemical_formula_weight         382.55
_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_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-11-20
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;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-11-20 deposited with the CCDC.
2016-02-10 downloaded from the CCDC.
;
_cell_angle_alpha                102.920(5)
_cell_angle_beta                 92.153(4)
_cell_angle_gamma                91.142(4)
_cell_formula_units_Z            2
_cell_length_a                   8.3642(4)
_cell_length_b                   9.4591(5)
_cell_length_c                   14.1094(8)
_cell_measurement_reflns_used    3638
_cell_measurement_temperature    150.02(10)
_cell_measurement_theta_max      28.3460
_cell_measurement_theta_min      3.8790
_cell_volume                     1086.82(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.02(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.871
_diffrn_measurement_details
;
  1 omega  -47.00   23.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -57.0000    0.0000 70

  2 omega  -17.00   61.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -99.0000  -60.0000 78

  3 omega  -17.00   61.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -99.0000   90.0000 78

  4 omega  -26.00   14.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -57.0000 -120.0000 40

  5 omega  -38.00   51.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663   57.0000 -180.0000 89

  6 omega  -79.00  -22.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663  -57.0000 -150.0000 57

  7 omega  -88.00   11.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663  -77.0000  -60.0000 99

  8 omega  -87.00    1.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663  -57.0000   30.0000 88

  9 omega  -86.00   -2.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663  -57.0000  120.0000 84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0491411000
_diffrn_orient_matrix_UB_12      -0.0576099000
_diffrn_orient_matrix_UB_13      -0.0277966000
_diffrn_orient_matrix_UB_21      0.0684322000
_diffrn_orient_matrix_UB_22      -0.0428414000
_diffrn_orient_matrix_UB_23      -0.0107432000
_diffrn_orient_matrix_UB_31      -0.0104803000
_diffrn_orient_matrix_UB_32      -0.0277404000
_diffrn_orient_matrix_UB_33      0.0421558000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_unetI/netI     0.0605
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.871
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15405
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.871
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.248
_diffrn_reflns_theta_min         3.243
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.073
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79470
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             418
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.280
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         5168
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0948
_refine_ls_R_factor_gt           0.0615
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0538P)^2^+0.4243P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1399
_refine_ls_wR_factor_ref         0.1566
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3535
_reflns_number_total             5168
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00039h2.cif
_cod_data_source_block           L8
_cod_depositor_comments
'Adding full bibliography for 7038378--7038379.cif.'
_cod_original_cell_volume        1086.81(10)
_cod_database_code               7038378
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         C21H23N7O6
_reflns_odcompleteness_completeness 99.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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:
 C22(H22A,H22B), C23(H23A,H23B), C27(H27A,H27B), C26(H26A,H26B), C24(H24A,
 H24B), C15(H15A,H15B), C25(H25A,H25B), C14(H14A,H14B), C17(H17A,H17B),
 C16(H16A,H16B), C18(H18A,H18B), C19(H19A,H19B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C6(H6), C9(H9), C4(H4), C12(H12), C11(H11)
2.c Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              6767
_olex2_date_sample_data_collection 2015-04-29
_olex2_submission_special_instructions 'No special instructions were received'