Nonlinear Optical Chromophores with Two Ferrocenyl, Octamethylferrocenyl, or 4-(Diphenylamino)phenyl Groups Attached to Rhenium(I) or Zinc(II) Centers
Coe, Benjamin J.; Foxon, Simon P.; Pilkington, Rachel A.; Sánchez, Sergio; Whittaker, Daniel; Clays, Koen; Depotter, Griet; Brunschwig, Bruce S.; Organometallics 34 (2015) 1701–; doi:10.1021/acs.organomet.5b00193

data_4087500
_publ_section_title
;
 Nonlinear Optical Chromophores with Two Ferrocenyl, Octamethylferrocenyl,
 or 4-(Diphenylamino)phenyl Groups Attached to Rhenium(I) or Zinc(II)
 Centers
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_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              1701
_journal_paper_doi               10.1021/acs.organomet.5b00193
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C38 H34 Fe2 N2 O4 Zn, C H Cl3'
_chemical_formula_sum            'C39 H35 Cl3 Fe2 N2 O4 Zn'
_chemical_formula_weight         879.11
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-05-22
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                84.808(2)
_cell_angle_beta                 73.656(2)
_cell_angle_gamma                84.961(2)
_cell_formula_units_Z            2
_cell_length_a                   9.8429(3)
_cell_length_b                   12.5224(3)
_cell_length_c                   15.4312(4)
_cell_measurement_reflns_used    7379
_cell_measurement_temperature    100
_cell_measurement_theta_max      68.38
_cell_measurement_theta_min      3.55
_cell_volume                     1813.77(9)
_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
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0758
_diffrn_reflns_av_unetI/netI     0.0756
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21512
_diffrn_reflns_theta_full        66.58
_diffrn_reflns_theta_max         66.58
_diffrn_reflns_theta_min         2.99
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.494
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.2889
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1565 before and 0.0831 after correction.
The Ratio of minimum to maximum transmission is 0.3836.
The \l/2 correction factor is 0.0000.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.990
_refine_diff_density_min         -1.634
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         6173
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0751
_refine_ls_R_factor_gt           0.0618
_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^)+(0.1225P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1636
_refine_ls_wR_factor_ref         0.1735
_reflns_number_gt                5028
_reflns_number_total             6173
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00193_si_003.cif
_cod_data_source_block           4.CHCl3
_cod_original_cell_volume        1813.78(8)
_cod_database_code               4087500
_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. Uiso/Uaniso restraints and constraints
Uanis(C22) = Uanis(C2) = Uanis(C5) = Uanis(C10) = Uanis(C35) = Uanis(C29)
3.a Ternary CH refined with riding coordinates:
 C39(H39)
3.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C1(H1), C2(H2), C4(H4), C22(H22), C21(H21), C19(H19), C23(H23),
 C24(H24), C26(H26), C27(H27), C28(H28), C30(H30), C34(H34), C33(H33), C32(H32),
  C31(H31), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12), C9(H9), C13(H13),
 C15(H15), C16(H16), C17(H17), C29(H29)
3.c Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C38(H38A,H38B,H38C)
;