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_7032783
_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         'C27 H19 N5 O2 Re, F6 P, H2 O'
_chemical_formula_sum            'C27 H21 F6 N5 O3 P Re'
_chemical_formula_weight         794.66
_chemical_name_systematic
;
 ? 
;
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 104.4190(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.9820(2)
_cell_length_b                   8.17950(10)
_cell_length_c                   24.0881(4)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.60
_cell_measurement_theta_min      3.341
_cell_volume                     2668.08(7)
_computing_cell_refinement
;
SAINT (2013) V8.34A; Integration Software for Single Crystal Data.
Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_data_collection
;
APEX 2 (2013) Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_data_reduction
;
SAINT (2013) V8.34A; Integration Software for Single Crystal Data.
Bruker AXS Inc., Madison, WI 53719-1173.
;
_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(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_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  0.0274
_diffrn_reflns_av_unetI/netI     0.0091
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            99183
_diffrn_reflns_theta_full        71.16
_diffrn_reflns_theta_max         71.16
_diffrn_reflns_theta_min         3.34
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.237
_exptl_absorpt_correction_T_max  0.7534
_exptl_absorpt_correction_T_min  0.4202
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.978
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.453
_refine_diff_density_min         -1.267
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         5025
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_gt           0.0263
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0334P)^2^+10.6351P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0654
_reflns_number_gt                5013
_reflns_number_total             5025
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt03077j2.cif
_cod_data_source_block           BALA33_0m
_cod_depositor_comments
'Adding full bibliography for 7032783--7032784.cif.'
_cod_database_code               7032783
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O3(H3A,H3B)
2.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C7(H7), C15(H15), C12(H12), C13(H13), C14(H14), C18(H18), C1(H1),
 C2(H2), C3(H3), C4(H4), C24(H24), C25(H25), C21(H21), C22(H22)
2.c Fitted hexagon refined as free rotating group:
 C9(C10,N2,C6,C7,C8), C15(N3,C11,C12,C13,C14), C5(N1,C1,C2,C3,C4), C24(C25,N5,
 C21,C22,C23)
;
_olex2_submission_special_instructions 'No special instructions were received'