Preparation and reactivity of a Ru(0) phosphino-carbene complex.
Mosaferi, Eliar; Pan, Li; Wang, Tongen; Sun, Yunshan; Pranckevicius, Conor; Stephan, Douglas W.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 1354–1358; doi:10.1039/c5dt04337a

data_7037842
_publ_section_title
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 Preparation and reactivity of a Ru(0) phosphino-carbene complex.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1354
_journal_page_last               1358
_journal_paper_doi               10.1039/c5dt04337a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety
'2(C25 H46 N4 O P2 Ru), C H2 Cl2, C6 H6, 2(Cl), 0.5(C5 H12)'
_chemical_formula_sum            'C59.5 H106 Cl4 N8 O2 P4 Ru2'
_chemical_formula_weight         1433.39
_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'
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-07-19
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-07-19 deposited with the CCDC.
2016-01-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.842(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5609(8)
_cell_length_b                   28.1621(19)
_cell_length_c                   23.5527(15)
_cell_measurement_reflns_used    9916
_cell_measurement_temperature    149
_cell_measurement_theta_max      27.29
_cell_measurement_theta_min      2.45
_cell_volume                     7667.4(9)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      149.31
_diffrn_measured_fraction_theta_full 0.9981
_diffrn_measured_fraction_theta_max 0.9981
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0993
_diffrn_reflns_av_unetI/netI     0.1162
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            59701
_diffrn_reflns_theta_full        27.4883
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.45
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.658
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6781
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0575 before and 0.0507 after correction.
The Ratio of minimum to maximum transmission is 0.9095.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.2416
_exptl_crystal_description       needle
_exptl_crystal_F_000             2998.8531
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.8811
_refine_diff_density_min         -1.6891
_refine_diff_density_rms         0.2789
_refine_ls_d_res_high            0.7699
_refine_ls_d_res_low             14.0810
_refine_ls_goodness_of_fit_ref   1.0441
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    160
_refine_ls_number_parameters     713
_refine_ls_number_reflns         17544
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0441
_refine_ls_R_factor_all          0.1240
_refine_ls_R_factor_gt           0.0620
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0786P)^2^+12.8195P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1521
_refine_ls_wR_factor_ref         0.1804
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -15
_reflns_limit_k_max              36
_reflns_limit_k_min              0
_reflns_limit_l_max              30
_reflns_limit_l_min              -12
_reflns_number_gt                10694
_reflns_number_total             17544
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c5dt04337a2.cif
_cod_data_source_block           lp003_0m
_cod_depositor_comments
'Adding full bibliography for 7037841--7037844.cif.'
_cod_database_code               7037842
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C55(0.5) H55a(0.5) H55b(0.5) H55c(0.5) C54(0.5) H54a(0.5)
 H54b(0.5) C53(0.5) H53a(0.5) H53b(0.5) C52(0.5) H52a(0.5) H52b(0.5) C51(0.5)
 H51a(0.5) H51b(0.5) H51c(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C62(H62a,H62b), C54(H54a,H54b), C53(H53a,H53b), C52(H52a,H52b)
3.b Me refined with riding coordinates:
 C1(H1a,H1b,H1c), C9(H9a,H9b,H9c), C11(H11a,H11b,H11c), C5(H5a,H5b,H5c),
 C30(H30a,H30b,H30c), C35(H35a,H35b,H35c), C36(H36a,H36b,H36c), C14(H14a,H14b,
 H14c), C38(H38a,H38b,H38c), C42(H42a,H42b,H42c), C46(H46a,H46b,H46c), C6(H6a,
 H6b,H6c), C48(H48a,H48b,H48c), C34(H34a,H34b,H34c), C15(H15a,H15b,H15c),
 C32(H32a,H32b,H32c), C7(H7a,H7b,H7c), C21(H21a,H21b,H21c), C13(H13a,H13b,H13c),
  C18(H18a,H18b,H18c), C26(H26a,H26b,H26c), C31(H31a,H31b,H31c), C17(H17a,H17b,
 H17c), C43(H43a,H43b,H43c), C47(H47a,H47b,H47c), C19(H19a,H19b,H19c), C44(H44a,
 H44b,H44c), C10(H10a,H10b,H10c), C55(H55a,H55b,H55c), C51(H51a,H51b,H51c)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C28(H28), C23(H23), C39(H39), C22(H22), C2(H2), C27(H27), C40(H40),
 C60(H60), C56(H56), C59(H59), C57(H57), C61(H61), C58(H58)
;
_olex2_submission_special_instructions 'No special instructions were received'