Synthesis of discrete Re(I) di- and tricarbonyl assemblies using a [4 ×1] directional bonding strategy.
Laramée-Milette, Baptiste; Lachance-Brais, Christophe; Hanan, Garry S.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 41–45; doi:10.1039/c4dt03077j

data_7032784
_publ_section_title
;
 Synthesis of discrete Re(I) di- and tricarbonyl assemblies using a [4
 \\times 1] directional bonding strategy.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              41
_journal_page_last               45
_journal_paper_doi               10.1039/c4dt03077j
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C88 H56 N16 O8 Re4, 4(F6 P)'
_chemical_formula_sum            'C88 H56 F24 N16 O8 P4 Re4'
_chemical_formula_weight         2790.21
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 94.010(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.917(16)
_cell_length_b                   12.514(7)
_cell_length_c                   32.083(17)
_cell_measurement_reflns_used    2011
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      35.265
_cell_measurement_theta_min      2.761
_cell_volume                     11181(11)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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    'XT (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_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  0.1522
_diffrn_reflns_av_unetI/netI     0.1580
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            9905
_diffrn_reflns_theta_full        16.11
_diffrn_reflns_theta_max         16.11
_diffrn_reflns_theta_min         1.27
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    9.638
_exptl_absorpt_correction_T_max  0.7472
_exptl_absorpt_correction_T_min  0.3258
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1469 before and 0.1067 after correction.
The Ratio of minimum to maximum transmission is 0.4360.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.658
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5344
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.110
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     589
_refine_ls_number_reflns         2641
_refine_ls_number_restraints     673
_refine_ls_restrained_S_all      2.219
_refine_ls_R_factor_all          0.1474
_refine_ls_R_factor_gt           0.0916
_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^)+(0.1700P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2344
_refine_ls_wR_factor_ref         0.2646
_reflns_number_gt                1384
_reflns_number_total             2641
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt03077j2.cif
_cod_data_source_block           BALA30_0m
_cod_depositor_comments
'Adding full bibliography for 7032783--7032784.cif.'
_cod_database_code               7032784
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C2-C1 = C1-C4 = C4-C3 = C3-C5 = C5-N1 = N1-C2
 1.39 with sigma of 0.02
 C6-C7 = C7-C8 = C8-C9 = C9-C10 = C10-N2 = N2-C6
 1.39 with sigma of 0.02
 C11-C12 = C12-C13 = C13-C14 = C14-C15 = C15-N3 = N3-C11
 1.39 with sigma of 0.02
 C26-C27 = C27-C28 = C28-C29 = C29-C30 = C30-N6 = N6-C26
 1.39 with sigma of 0.02
 C2-C3 = C1-C5 = C4-N1
 2.78 with sigma of 0.02
 C6-C9 = C7-C10 = C8-N2
 2.78 with sigma of 0.02
 C11-C14 = C12-C15 = C13-N3
 2.78 with sigma of 0.02
 C31-C34 = C32-C35 = C33-N7
 2.78 with sigma of 0.02
 C26-C29 = C27-C30 = C28-N6
 2.78 with sigma of 0.02
 C2-C4 = C1-C3 = C4-C5 = C3-N1 = C5-C2
 2.41 with sigma of 0.04
 C6-C8 = C7-C9 = C8-C10 = C9-N2 = C10-C6
 2.41 with sigma of 0.04
 C11-C13 = C12-C14 = C13-C15 = C14-N3 = C15-C11
 2.41 with sigma of 0.04
 C31-C33 = C32-C34 = C33-C35 = C34-N7 = C35-C31
 2.41 with sigma of 0.04
 C26-C28 = C27-C29 = C28-C30 = C29-N6 = C30-C26
 2.41 with sigma of 0.04
 P2-F7 \\sim P2-F8 \\sim P2-F9 \\sim P2-F10 \\sim P2-F11 \\sim P2-F12
 with sigma of 0.02
3. Restrained planarity
 C17, C20, N4, C19, C16, C18
 with sigma of 0.1
 N2, C6, C7, C8, C9, C10
 with sigma of 0.1
 C11, C12, C13, C14, C15, N3
 with sigma of 0.1
4. Rigid bond restraints
 C2, C1, C4, C3, C5, N1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C44, O4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C43, O3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C6, C7, C8, C9, C10, N2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C11, C12, C13, C14, C15, N3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C31, C32, C33, C34, C35, N7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C26, C27, C28, C29, C30, N6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N5, C25, C24, C23, C22, C21
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C17, C20, N4, C19, C16, C18
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C40, N8, C36, C37, C39, C38
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O2, C42, Re1, O1, C41
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1, C2, C3, C4, C5, N1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C14, C13, C12, C11, N3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 P1, F5, F1, F6, F2, F4, F3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 P2, F7, F12, F8, F10, F11, F9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C44 \\sim O4: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C43 \\sim O3: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C40 \\sim N8 \\sim C36 \\sim C37 \\sim C39 \\sim C38: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
C17 \\sim C20 \\sim N4 \\sim C19 \\sim C16 \\sim C18: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
C2 \\sim C1 \\sim C4 \\sim C3 \\sim C5 \\sim N1: within 1.7A with sigma of 0.04
and sigma for terminal atoms of 0.08
C6 \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim N2: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim N3: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim N7: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim N6: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
N5 \\sim C25 \\sim C24 \\sim C23 \\sim C22 \\sim C21: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
Re1 \\sim O1 \\sim O2 \\sim C41 \\sim C42: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim N1: within 1.7A with sigma of 0.04
and sigma for terminal atoms of 0.08
C14 \\sim C13 \\sim C12 \\sim C11 \\sim N3: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
P1 \\sim F5 \\sim F1 \\sim F6 \\sim F2 \\sim F4 \\sim F3: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
P2 \\sim F7 \\sim F12 \\sim F8 \\sim F10 \\sim F11 \\sim F9: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(N4) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(C44)
\\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(N3) \\sim Ueq,
Uanis(N8) \\sim Ueq, Uanis(N6) \\sim Ueq: with sigma of 0.03 and sigma for
terminal atoms of 0.02
Uanis(N2) \\sim Ueq: with sigma of 0.015 and sigma for terminal atoms of 0.03
6.a Aromatic/amide H refined with riding coordinates:
 C24(H24), C23(H23), C22(H22), C21(H21), C35(H35), C34(H34), C33(H33),
 C32(H32), C36(H36), C37(H37), C39(H39), C40(H40), C29(H29), C27(H27), C1(H1),
 C2(H2), C3(H3), C4(H4), C17(H17), C16(H16), C20(H20), C19(H19), C13(H13),
 C12(H12), C15(H15), C9(H9), C14(H14), C7(H7)
6.b Fitted hexagon refined as free rotating group:
 N5(C25,C24,C23,C22,C21), N7(C35,C34,C33,C32,C31), N8(C36,C37,C38,C39,C40),
 C1(C2,C3,C4,C5,N1), C18(C17,C16,N4,C20,C19)
;
_olex2_submission_special_instructions 'No special instructions were received'