Synthesis, structures, and reactivity of isomers of [RuCp*(1,4-(Me<sub>2</sub>N)<sub>2</sub>C<sub>6</sub>H<sub>4</sub>)]<sub>2</sub>.
Longhi, Elena; Risko, Chad; Bacsa, John; Khrustalev, Victor; Rigin, Sergei; Moudgil, Karttikay; Timofeeva, Tatiana V.; Marder, Seth R.; Barlow, Stephen; Dalton transactions (Cambridge, England : 2003) 50 (2021) 13020–13030; doi:10.1039/d1dt02155a

data_7708134
_publ_section_title
;
 Synthesis, structures, and reactivity of isomers of
 [RuCp*(1,4-(Me<sub>2</sub>N)<sub>2</sub>C<sub>6</sub>H<sub>4</sub>)]<sub>2</sub>.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13020
_journal_page_last               13030
_journal_paper_doi               10.1039/d1dt02155a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C40 H62 N4 Ru2'
_chemical_formula_sum            'C40 H62 N4 Ru2'
_chemical_formula_weight         801.073
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-15
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-05-15 deposited with the CCDC.	2021-08-17 downloaded from the CCDC.
;
_cell_angle_alpha                89.304(1)
_cell_angle_beta                 79.584(1)
_cell_angle_gamma                72.407(1)
_cell_formula_units_Z            2
_cell_length_a                   10.6226(1)
_cell_length_b                   12.2061(2)
_cell_length_c                   15.1648(1)
_cell_measurement_reflns_used    38690
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      38.4010
_cell_measurement_theta_min      2.0710
_cell_volume                     1841.53(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement
'olex2.refine 1.3-alpha (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9994
_diffrn_measured_fraction_theta_max 0.9992
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -52.00 -20.00   0.50    3.00    --  -22.41  98.00  20.00   64
  2  \w     16.00  85.00   0.50    3.00    --   22.41  57.00 -30.00  138
  3  \w     21.00  48.00   0.50    3.00    --   22.41  38.00-180.00   54
  4  \w    -10.00  15.00   0.50    3.00    --   22.41 -98.00 -86.00   50
  5  \w    -24.00  53.00   0.50    3.00    --   22.41 -99.00-120.00  154
  6  \w    -48.00  28.00   0.50    3.00    --   22.41 -38.00  30.00  152
  7  \w     36.00  79.00   0.50    3.00    --   22.41-178.00  90.00   86
  8  \w    -91.00  -3.00   0.50    3.00    --  -22.41 -77.00-120.00  176
  9  \w    -93.00  -3.00   0.50    3.00    --  -22.41 -77.00   0.00  180
 10  \w    -93.00 -34.00   0.50    3.00    --  -22.41 -77.00 150.00  118
 11  \w    -93.00  -3.00   0.50    3.00    --  -22.41 -77.00 120.00  180
 12  \w     43.00  71.00   0.50    3.00    --   22.41 178.00-150.00   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0067709000
_diffrn_orient_matrix_UB_12      0.0296996000
_diffrn_orient_matrix_UB_13      0.0379230000
_diffrn_orient_matrix_UB_21      0.0607708000
_diffrn_orient_matrix_UB_22      0.0067439000
_diffrn_orient_matrix_UB_23      -0.0240939000
_diffrn_orient_matrix_UB_31      -0.0366535000
_diffrn_orient_matrix_UB_32      0.0528815000
_diffrn_orient_matrix_UB_33      -0.0157358000
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_Laue_measured_fraction_full 0.9994
_diffrn_reflns_Laue_measured_fraction_max 0.9992
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            55488
_diffrn_reflns_point_group_measured_fraction_full 0.9994
_diffrn_reflns_point_group_measured_fraction_max 0.9992
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         36.32
_diffrn_reflns_theta_min         1.75
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.853
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.397
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_description       prism
_exptl_crystal_F_000             831.219
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.337
_exptl_crystal_size_mid          0.251
_exptl_crystal_size_min          0.164
_refine_diff_density_max         0.6807
_refine_diff_density_min         -0.4334
_refine_diff_density_rms         0.1049
_refine_ls_d_res_high            0.6001
_refine_ls_d_res_low             11.6232
_refine_ls_goodness_of_fit_ref   1.0275
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     1023
_refine_ls_number_reflns         17857
_refine_ls_number_restraints     1041
_refine_ls_restrained_S_all      0.9971
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0251
_refine_ls_shift/su_max          0.0007
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0253P)^2^+0.0571P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0567
_refine_ls_wR_factor_ref         0.0586
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              20
_reflns_limit_k_min              -20
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                15504
_reflns_number_total             17857
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d1dt02155a2.cif
_cod_data_source_block           EL-II-66
_cod_depositor_comments
'Adding full bibliography for 7708131--7708134.cif.'
_cod_database_code               7708134
_chemical_oxdiff_formula         'C80  H124  N8  Ru4  '
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.23
_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. Rigid body (RIGU) restrains
 C19, C20, C23, C21, C22, C28, H28a, H28b, H28c, C27, H27a, H27c, C25, H25a,
 H25b, H25c, C24, H24a, H24b, H24c, C26, H26c, H27b, H26a, H26b
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.02
 Ru1, N4, N2, N1, N3, C31, C11, H11, C32, C1, C6, C12, C33, C9, H9, C10, H10,
 C5, H5, C17, H17, C4, H4, C35, C18, H18, C16, H16, C13, C29, H29a, H29b, H29c,
 C30, H30b, C39, H39a, H39b, C40, H40a, H40b, C38, H38a, H38b, H38c, C8, H8a,
 H8b, H8c, C2, H2a, H2b, H2c, C14, H14a, H14b, H14c, C3, H3a, H3b, H3c, C15,
 H15a, H15b, H15c, C34, C7, H30c, H39c, H40c, H36b, H7a, H7b, H7c, C36, H36c,
 H36a, C37, H37a, H37b, H37c, H30a
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.02
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a loop with paratone oil'
_olex2_submission_original_sample_id EL-II-66
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.266
_oxdiff_exptl_absorpt_empirical_full_min 0.849