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_4088895
_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         'C29 H17 N5 O3 Re, C F3 O3 S, C2 H3 N'
_chemical_formula_sum            'C32 H20 F3 N6 O6 Re S'
_chemical_formula_weight         859.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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                90
_cell_angle_beta                 102.651(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9062(5)
_cell_length_b                   15.4034(4)
_cell_length_c                   16.6113(5)
_cell_measurement_reflns_used    4443
_cell_measurement_temperature    150.04(18)
_cell_measurement_theta_max      26.2450
_cell_measurement_theta_min      3.3780
_cell_volume                     3721.5(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.04(18)
_diffrn_detector_area_resol_mean 8.0714
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
  1 omega   -2.00   89.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       19.6440   57.0000 -150.0000 91

  2 omega  -11.00   89.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       19.6440   77.0000   90.0000 100
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0396511000
_diffrn_orient_matrix_UB_12      -0.0047726000
_diffrn_orient_matrix_UB_13      0.0322383000
_diffrn_orient_matrix_UB_21      0.0267693000
_diffrn_orient_matrix_UB_22      -0.0086755000
_diffrn_orient_matrix_UB_23      -0.0295402000
_diffrn_orient_matrix_UB_31      0.0093119000
_diffrn_orient_matrix_UB_32      0.0449729000
_diffrn_orient_matrix_UB_33      -0.0022438000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_unetI/netI     0.0798
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            13112
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.384
_diffrn_reflns_theta_min         3.104
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.384
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_description       needle
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.3455
_exptl_crystal_size_mid          0.0765
_exptl_crystal_size_min          0.0755
_refine_diff_density_max         4.678
_refine_diff_density_min         -1.619
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         7541
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0585
_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^)+(0.0722P)^2^+16.0526P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1485
_refine_ls_wR_factor_ref         0.1667
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5604
_reflns_number_total             7541
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00536_si_002.cif
_cod_data_source_block           6.MeCN
_cod_database_code               4088895
_chemical_oxdiff_formula         ReC30H25O6SF3N5
_reflns_odcompleteness_completeness 98.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C9(H9), C4(H4), C15(H15), C22(H22), C10(H10), C19(H19), C18(H18),
 C21(H21), C16(H16), C7(H7), C2(H2), C12(H12), C13(H13)
2.b Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C28(H28A,H28B,H28C)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2013-12-02
_olex2_submission_special_instructions 'No special instructions were received'