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_4088890
_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         'C15 H6 Cl N4 O3 Re, C3 H6 O'
_chemical_formula_sum            'C18 H12 Cl N4 O4 Re'
_chemical_formula_weight         569.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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                90.00
_cell_angle_beta                 100.237(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.7065(4)
_cell_length_b                   24.7860(10)
_cell_length_c                   12.0178(6)
_cell_measurement_reflns_used    2558
_cell_measurement_temperature    100.7(9)
_cell_measurement_theta_max      27.0700
_cell_measurement_theta_min      3.1090
_cell_volume                     1965.89(18)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.7(9)
_diffrn_detector_area_resol_mean 8.3367
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -73.00  -20.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.1131  -77.0000 -150.0000 53

  2 omega  -25.00   28.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.1131  -99.0000   90.0000 53

  3 omega  -16.00  102.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       20.5194   37.0000   90.0000 118
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0018484000
_diffrn_orient_matrix_UB_12      -0.0223400000
_diffrn_orient_matrix_UB_13      0.0366453000
_diffrn_orient_matrix_UB_21      -0.1073712000
_diffrn_orient_matrix_UB_22      0.0012899000
_diffrn_orient_matrix_UB_23      -0.0089468000
_diffrn_orient_matrix_UB_31      -0.0054626000
_diffrn_orient_matrix_UB_32      -0.0178426000
_diffrn_orient_matrix_UB_33      -0.0465871000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_unetI/netI     0.0890
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6760
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.01
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.349
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47895
_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            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.926
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.822
_refine_diff_density_min         -1.394
_refine_diff_density_rms         0.244
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         3596
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0544
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0405P)^2^+7.4761P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1145
_refine_ls_wR_factor_ref         0.1249
_reflns_number_gt                2824
_reflns_number_total             3596
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00536_si_002.cif
_cod_data_source_block           1.Me2CO
_cod_original_cell_volume        1965.87(18)
_cod_database_code               4088890
_chemical_oxdiff_formula         'Re Cl1 C18 H12 N4 O4'
_chemical_oxdiff_usercomment     'Red Rhombohedron 0.1 0.1 0.05'
_reflns_odcompleteness_completeness 99.84
_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 planarity
 C16, C17, O4, C18
 with sigma of 0.1
3. Rigid bond restraints
 C15
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C18, O4, C17, C16
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C15: within 1.7A with sigma of 0.005 and sigma for terminal atoms of 0.1
C17 \\sim C16 \\sim C18 \\sim O4: within 1.7A with sigma of 0.005 and sigma for
terminal atoms of 0.1
Uanis(C18) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C16)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.04
Uanis(C15) = Uanis(C13) = Uanis(C14)
Uanis(C9) = Uanis(C8) = Uanis(C7) = Uanis(C6) = Uanis(C10)
Uanis(C16) = Uanis(C18)
5.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C7(H7), C4(H4), C9(H9), C1(H1), C2(H2)
5.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C16(H16A,H16B,H16C)
;
_olex2_date_sample_data_collection 1361196625.7
_olex2_submission_special_instructions 'No special instructions were received'