Rhenium(I) Tricarbonyl Complexes with Peripheral N-Coordination Sites: A Foundation for Heterotrimetallic Nonlinear Optical Chromophores
Coe, Benjamin J.; Foxon, Simon P.; Pilkington, Rachel A.; Sánchez, Sergio; Whittaker, Daniel; Clays, Koen; Van Steerteghem, Nick; Brunschwig, Bruce S.; Organometallics 35 (2016) 3014–; doi:10.1021/acs.organomet.6b00536

data_4088891
_publ_section_title
;
 Rhenium(I) Tricarbonyl Complexes with Peripheral N-Coordination Sites: A
 Foundation for Heterotrimetallic Nonlinear Optical Chromophores
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              3014
_journal_paper_doi               10.1021/acs.organomet.6b00536
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C17 H9 N5 O3 Re, C F3 O3 S, C7 H8'
_chemical_formula_sum            'C25 H17 F3 N5 O6 Re S'
_chemical_formula_weight         758.70
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-06-20
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                70.788(5)
_cell_angle_beta                 80.269(4)
_cell_angle_gamma                76.658(4)
_cell_formula_units_Z            2
_cell_length_a                   9.8664(5)
_cell_length_b                   10.8251(6)
_cell_length_c                   13.6341(7)
_cell_measurement_reflns_used    4793
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.6620
_cell_measurement_theta_min      2.9400
_cell_volume                     1331.09(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8.3367
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -55.00   32.00   1.0000   22.9100
omega____ theta____ kappa____ phi______ frames
    -      -21.7931   77.0000 -150.0000 87

  2 omega  -12.00  104.00   1.0000   22.9100
omega____ theta____ kappa____ phi______ frames
    -       23.1993   77.0000   60.0000 116

  3 omega    2.00   42.00   1.0000   22.9100
omega____ theta____ kappa____ phi______ frames
    -       23.1993   77.0000  150.0000 40

  4 omega   82.00  117.00   1.0000   22.9100
omega____ theta____ kappa____ phi______ frames
    -       23.1993   77.0000  150.0000 35

  5 omega    0.00  120.00   1.0000   22.9100
omega____ theta____ kappa____ phi______ frames
    -       23.1993   77.0000  -60.0000 120
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0469329000
_diffrn_orient_matrix_UB_12      0.0089229000
_diffrn_orient_matrix_UB_13      -0.0462414000
_diffrn_orient_matrix_UB_21      0.0572182000
_diffrn_orient_matrix_UB_22      -0.0314101000
_diffrn_orient_matrix_UB_23      0.0303304000
_diffrn_orient_matrix_UB_31      -0.0062419000
_diffrn_orient_matrix_UB_32      -0.0626518000
_diffrn_orient_matrix_UB_33      -0.0029040000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0686
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9086
_diffrn_reflns_theta_full        26.73
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         2.93
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.715
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36663
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.893
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.122
_refine_diff_density_min         -2.195
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         5640
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0285P)^2^+0.3276P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0808
_refine_ls_wR_factor_ref         0.0865
_reflns_number_gt                5103
_reflns_number_total             5640
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00536_si_002.cif
_cod_data_source_block           2.PhMe
_cod_original_cell_volume        1331.09(12)
_cod_database_code               4088891
_chemical_oxdiff_formula         'Re C20 N5 O3 F3 S1'
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.67
_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. Uiso/Uaniso restraints and constraints
Uanis(N5) \\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of 0.006 and sigma for
terminal atoms of 0.012
Uanis(C13) = Uanis(C14) = Uanis(C15)
3.a Me refined with riding coordinates:
 C17(H17A,H17B,H17C), C19(H19A,H19B,H19C)
3.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C23(H23), C22(H22), C9(H9), C25(H25), C1(H1), C2(H2), C24(H24),
 C21(H21), C7(H7), C4(H4)
;
_olex2_submission_special_instructions 'No special instructions were received'