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_4088892
_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         'C20 H11 N5 O3 Re, C F3 O3 S, 0.5(C7 H8)'
_chemical_formula_sum            'C24.5 H15 F3 N5 O6 Re S'
_chemical_formula_weight         750.67
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.9198(11)
_cell_length_b                   14.1928(6)
_cell_length_c                   18.5858(8)
_cell_measurement_reflns_used    4162
_cell_measurement_temperature    150.04(13)
_cell_measurement_theta_max      26.7630
_cell_measurement_theta_min      3.4410
_cell_volume                     5518.3(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.04(13)
_diffrn_detector_area_resol_mean 5.1852
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.828
_diffrn_measurement_details
;
  1 omega    3.00   67.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.7722    0.0000 -120.0000 64

  2 omega  -74.00  -29.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.7722    0.0000 -120.0000 45
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0085639000
_diffrn_orient_matrix_UB_12      -0.0294741000
_diffrn_orient_matrix_UB_13      -0.0292614000
_diffrn_orient_matrix_UB_21      0.0327910000
_diffrn_orient_matrix_UB_22      -0.0083779000
_diffrn_orient_matrix_UB_23      -0.0072719000
_diffrn_orient_matrix_UB_31      -0.0005553000
_diffrn_orient_matrix_UB_32      -0.0394957000
_diffrn_orient_matrix_UB_33      0.0233990000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_av_unetI/netI     0.1086
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.828
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15277
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.828
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.636
_diffrn_reflns_theta_min         3.073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.548
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.807
_exptl_crystal_description       needle
_exptl_crystal_F_000             2904
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.273
_refine_diff_density_min         -1.245
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         5876
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.1122
_refine_ls_R_factor_gt           0.0526
_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^)+(0.0156P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0747
_refine_ls_wR_factor_ref         0.1011
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3534
_reflns_number_total             5876
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00536_si_002.cif
_cod_data_source_block           3.0.5PhMe
_cod_original_formula_sum        'C24.50 H15 F3 N5 O6 Re S'
_cod_database_code               4088892
_chemical_oxdiff_formula         'C21 H11 N5 F3 Cl4 O6 Re S'
_reflns_odcompleteness_completeness 98.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_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
 C22-C29
 2.5429 with sigma of 0.02
 C28-C22
 2.5429 with sigma of 0.02
 C22-C24
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N3 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim C20: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
C24 \\sim C29 \\sim C26 \\sim C25 \\sim C27 \\sim C28 \\sim C22: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 C22, C24, C28, C27, C26, C25, C29
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C22(0.5) H22A(0.5) H22B(0.5) H22C(0.5) C27(0.5) H27(0.5) C28(0.5)
 H28(0.5) C24(0.5) C29(0.5) H29(0.5) C25(0.5) H25(0.5) C26(0.5) H26(0.5)
6.a Me refined with riding coordinates:
 C22(H22A,H22B,H22C)
6.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C10(H10), C4(H4), C2(H2), C1(H1), C16(H16), C17(H17),
 C18(H18), C19(H19), C20(H20), C27(H27), C28(H28), C29(H29), C25(H25), C26(H26)
6.c Fitted hexagon refined as free rotating group:
 C27(C28,C24,C29,C25,C26)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2013-11-12
_olex2_submission_special_instructions 'No special instructions were received'