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_4088893
_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         'C21 H10 N6 O3 Re, C F3 O3 S, 0.5(C3 O)'
_chemical_formula_sum            'C23.5 H13 F3 N6 O6.5 Re S'
_chemical_formula_weight         758.66
_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
_audit_creation_date             2016-06-14
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                89.784(6)
_cell_angle_beta                 66.738(8)
_cell_angle_gamma                67.606(8)
_cell_formula_units_Z            2
_cell_length_a                   10.6015(10)
_cell_length_b                   12.0951(9)
_cell_length_c                   12.4270(8)
_cell_measurement_reflns_used    3435
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      25.3710
_cell_measurement_theta_min      3.3580
_cell_volume                     1333.2(2)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector_area_resol_mean 10.3705
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
  1 omega  -34.00   55.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.6555   57.0000    0.0000 89

  2 omega  -82.00   13.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.6555  -57.0000 -150.0000 95

  3 omega   34.00  100.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       11.6555 -178.0000 -150.0000 66
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0659413000
_diffrn_orient_matrix_UB_12      0.0102316000
_diffrn_orient_matrix_UB_13      -0.0143485000
_diffrn_orient_matrix_UB_21      0.0140119000
_diffrn_orient_matrix_UB_22      -0.0055304000
_diffrn_orient_matrix_UB_23      -0.0608885000
_diffrn_orient_matrix_UB_31      -0.0430130000
_diffrn_orient_matrix_UB_32      0.0633355000
_diffrn_orient_matrix_UB_33      0.0080755000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_unetI/netI     0.0968
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8303
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.347
_diffrn_reflns_theta_min         3.285
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.710
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56713
_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 light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.890
_exptl_crystal_description       needle
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.105
_refine_diff_density_min         -0.858
_refine_diff_density_rms         0.194
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         4838
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0472
_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^)+(0.0220P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0762
_refine_ls_wR_factor_ref         0.0853
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4013
_reflns_number_total             4838
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00536_si_002.cif
_cod_data_source_block           4.0.5Me2CO
_cod_original_formula_sum        'C23.50 H13 F3 N6 O6.50 Re S'
_cod_database_code               4088893
_chemical_oxdiff_formula         ReC25H10O4Sf3N6
_reflns_odcompleteness_completeness 98.66
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C22-C23 \\sim C23-C24
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C24 \\sim C22 \\sim O4 \\sim C23: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
4. Others
 Fixed Sof: O4(0.5) C22(0.5) C23(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C7(H7), C10(H10), C1(H1), C16(H16), C17(H17), C9(H9), C13(H13),
 C4(H4), C14(H14)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2013-11-27
_olex2_submission_special_instructions 'No special instructions were received'