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_4088894
_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         'C27 H14 Cl N4 O3 Re, C4 H4'
_chemical_formula_sum            'C31 H18 Cl N4 O3 Re'
_chemical_formula_weight         716.14
_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
_audit_creation_date             2016-06-08
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.193(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.0510(8)
_cell_length_b                   23.671(3)
_cell_length_c                   15.0206(15)
_cell_measurement_reflns_used    1415
_cell_measurement_temperature    150.04(18)
_cell_measurement_theta_max      23.3730
_cell_measurement_theta_min      3.3570
_cell_volume                     2505.2(5)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.04(18)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -77.00  -36.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.7892  126.0000  -79.0000 41

  2 omega  -88.00  -36.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.7892 -178.0000  -30.0000 52

  3 omega   10.00   78.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3360 -126.0000 -157.0000 68

  4 omega   17.00   92.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3360   77.0000 -120.0000 75

  5 omega  -35.00   66.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3360  -19.0000  -90.0000 101
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0073876000
_diffrn_orient_matrix_UB_12      -0.0141810000
_diffrn_orient_matrix_UB_13      0.0416167000
_diffrn_orient_matrix_UB_21      -0.0121082000
_diffrn_orient_matrix_UB_22      -0.0263061000
_diffrn_orient_matrix_UB_23      -0.0220970000
_diffrn_orient_matrix_UB_31      0.0996129000
_diffrn_orient_matrix_UB_32      -0.0021432000
_diffrn_orient_matrix_UB_33      -0.0039571000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1352
_diffrn_reflns_av_unetI/netI     0.2215
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14375
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         3.214
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.001
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79400
_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            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.899
_exptl_crystal_description       block
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.261
_refine_diff_density_min         -0.875
_refine_diff_density_rms         0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.948
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         5108
_refine_ls_number_restraints     236
_refine_ls_restrained_S_all      0.929
_refine_ls_R_factor_all          0.1554
_refine_ls_R_factor_gt           0.0751
_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.1240
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2889
_reflns_number_total             5108
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00536_si_002.cif
_cod_data_source_block           5.0.5PhMe
_cod_database_code               4088894
_chemical_oxdiff_formula         ReC30H30N4O3Cl
_reflns_odcompleteness_completeness 99.68
_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. Restrained distances
 C31-C34
 1.45 with sigma of 0.02
 C30-C34
 2.4 with sigma of 0.02
 C32-C34
 2.4 with sigma of 0.02
3. Restrained planarity
 C34, C31, C32, C33, C28, C29, C30
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C26 \\sim C27 \\sim C25: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C34 \\sim C31 \\sim C32 \\sim C33 \\sim C28 \\sim C29 \\sim C30: within 1.7A
with sigma of 0.002 and sigma for terminal atoms of 0.002
Uanis(O2) = Uanis(C26)
5. Rigid body (RIGU) restrains
 N4, C24, C18, C20, C17, C22, C21, C19, N2, C8, C9, C6, C7, C10, N1, C2, C5,
 C4, C3, C1, C11, C13, C15, C12, C23, C14, N3, C16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C26, O2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C34, C31, C30, C29, C28, C33, C32
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
6. Others
 Fixed Sof: C33(0.5) H33(0.5) C28(0.5) H28(0.5) C29(0.5) H29(0.5) C30(0.5)
 H30(0.5) C32(0.5) H32(0.5) C34(0.5) H34A(0.5) H34B(0.5) H34C(0.5)
7.a Me refined with riding coordinates:
 C34(H34A,H34B,H34C)
7.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C2(H2), C16(H16), C4(H4), C13(H13), C9(H9), C1(H1), C15(H15),
 C22(H22), C7(H7), C12(H12), C21(H21), C10(H10), C19(H19), C33(H33), C28(H28),
 C29(H29), C30(H30), C32(H32)
7.c Fitted hexagon refined as free rotating group:
 C33(C28,C29,C30,C31,C32)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2013-12-13
_olex2_submission_special_instructions 'No special instructions were received'