Ruthenaphosphaalkenyls: Synthesis, Structures, and Their Conversion to η2-Phosphaalkene Complexes
Greenacre, Victoria K.; Trathen, Nicola; Crossley, Ian R.; Organometallics 34 (2015) 2533–; doi:10.1021/om5012177

data_4085712
_publ_section_title
;
 Ruthenaphosphaalkenyls: Synthesis, Structures, and Their Conversion to
 \h2-Phosphaalkene Complexes
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2533
_journal_paper_doi               10.1021/om5012177
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C41 H40 Cl O P3 Ru Si, 2(C4 H10 O)'
_chemical_formula_sum            'C49 H60 Cl O3 P3 Ru Si'
_chemical_formula_weight         954.49
_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
_audit_creation_date             2014-11-24
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90
_cell_angle_beta                 95.201(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7961(5)
_cell_length_b                   34.2580(17)
_cell_length_c                   14.8457(7)
_cell_measurement_reflns_used    4709
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      70.6420
_cell_measurement_theta_min      3.9080
_cell_volume                     4961.6(4)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58)'
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58)'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean 16.1033
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0237960000
_diffrn_orient_matrix_UB_12      0.0444111000
_diffrn_orient_matrix_UB_13      -0.0039523000
_diffrn_orient_matrix_UB_21      0.0863763000
_diffrn_orient_matrix_UB_22      -0.0057515000
_diffrn_orient_matrix_UB_23      -0.0806805000
_diffrn_orient_matrix_UB_31      -0.1299816000
_diffrn_orient_matrix_UB_32      0.0043291000
_diffrn_orient_matrix_UB_33      -0.0657910000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0890
_diffrn_reflns_av_unetI/netI     0.1410
_diffrn_reflns_laue_measured_fraction_full 0.984
_diffrn_reflns_laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15639
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.680
_diffrn_reflns_theta_max         70.946
_diffrn_reflns_theta_min         3.256
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.491
_exptl_absorpt_correction_T_max  0.874
_exptl_absorpt_correction_T_min  0.489
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
'CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) Numerical absorption correction based on gaussian integration over a multifaceted crystal model'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_description
;
;
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.866
_refine_diff_density_min         -1.799
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         9180
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.1138
_refine_ls_R_factor_gt           0.0876
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1365P)^2^+7.2920P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2484
_refine_ls_wR_factor_ref         0.2864
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6502
_reflns_number_total             9180
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5012177_si_003.cif
_cod_data_source_block           compound_2
_cod_depositor_comments
'Adding full bibliography for 4085712--4085714.cif.'
_cod_database_code               4085712
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C45 H60 O3 Cl1 P3 Si1 Ru1'
_shelx_estimated_absorpt_t_max   0.877
_shelx_estimated_absorpt_t_min   0.337
_reflns_odcompleteness_completeness 98.41
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1(0.075) H2A(0.133) H2B(0.133) H2C(0.133) H3A(0.189) H3B(0.189)
 H3C(0.189) H4A(0.158) H4B(0.158) H4C(0.158) H7(0.094) H8(0.13) H9(0.093)
 H10(0.078) H11(0.067) H13(0.063) H14(0.082) H15(0.096) H16(0.087) H17(0.067)
 H19(0.08) H20(0.093) H21(0.105) H22(0.099) H23(0.077) H25(0.07) H26(0.089)
 H27(0.084) H28(0.077) H29(0.061) H31(0.048) H32(0.07) H33(0.069) H34(0.082)
 H35(0.062) H37(0.064) H38(0.073) H39(0.081) H40(0.081) H41(0.065) H1SA(0.296)
 H1SB(0.296) H2SA(0.489) H2SB(0.489) H2SC(0.489) H3SA(0.364) H3SB(0.364)
 H4SA(0.447) H4SB(0.447) H4SC(0.447) H5SA(0.304) H5SB(0.304) H6SA(0.335)
 H6SB(0.335) H6SC(0.335) H7SA(0.389) H7SB(0.389) H8SA(0.363) H8SB(0.363)
 H8SC(0.363)
 Fixed X: H1(0.2928) H2A(0.729) H2B(0.6592) H2C(0.7055) H3A(0.475) H3B(0.3256)
 H3C(0.4041) H4A(0.5702) H4B(0.5417) H4C(0.4163) H7(0.0699) H8(0.0364)
 H9(0.0736) H10(0.1534) H11(0.192) H13(0.4444) H14(0.5663) H15(0.4545)
 H16(0.2217) H17(0.1004) H19(-0.1131) H20(-0.3217) H21(-0.3299) H22(-0.132)
 H23(0.083) H25(0.4392) H26(0.3535) H27(0.1319) H28(0.0067) H29(0.0967)
 H31(0.5968) H32(0.8256) H33(0.8859) H34(0.7172) H35(0.49) H37(0.3417)
 H38(0.2387) H39(0.0918) H40(0.0473) H41(0.152) H1SA(0.305) H1SB(0.3788)
 H2SA(0.1891) H2SB(0.1039) H2SC(0.1773) H3SA(0.4939) H3SB(0.4214) H4SA(0.4673)
 H4SB(0.3764) H4SC(0.3057) H5SA(0.563) H5SB(0.6091) H6SA(0.7966) H6SB(0.7844)
 H6SC(0.8302) H7SA(0.425) H7SB(0.3843) H8SA(0.3826) H8SB(0.5397) H8SC(0.4988)
 Fixed Y: H1(0.6476) H2A(0.5995) H2B(0.5872) H2C(0.6314) H3A(0.565)
 H3B(0.5816) H3C(0.5545) H4A(0.6502) H4B(0.6828) H4C(0.6634) H7(0.5973)
 H8(0.5569) H9(0.4909) H10(0.4628) H11(0.5022) H13(0.5607) H14(0.5165)
 H15(0.482) H16(0.4921) H17(0.5358) H19(0.5622) H20(0.5768) H21(0.6135)
 H22(0.6394) H23(0.6265) H25(0.7669) H26(0.7865) H27(0.7684) H28(0.7263)
 H29(0.7043) H31(0.6725) H32(0.6896) H33(0.755) H34(0.8022) H35(0.786)
 H37(0.7194) H38(0.7575) H39(0.8085) H40(0.8197) H41(0.7824) H1SA(0.5103)
 H1SB(0.4856) H2SA(0.5128) H2SB(0.4909) H2SC(0.4662) H3SA(0.4411) H3SB(0.4652)
 H4SA(0.4049) H4SB(0.3888) H4SC(0.4129) H5SA(0.8864) H5SB(0.9248) H6SA(0.9006)
 H6SB(0.8595) H6SC(0.8977) H7SA(0.9078) H7SB(0.8653) H8SA(0.8641) H8SB(0.8775)
 H8SC(0.8354)
 Fixed Z: H1(0.726) H2A(0.6798) H2B(0.769) H2C(0.7554) H3A(0.5648) H3B(0.5788)
 H3C(0.6547) H4A(0.5344) H4B(0.6076) H4C(0.5469) H7(0.7877) H8(0.6628)
 H9(0.6705) H10(0.8097) H11(0.9391) H13(1.0083) H14(1.1061) H15(1.2128)
 H16(1.2236) H17(1.1269) H19(0.924) H20(0.979) H21(1.1109) H22(1.1791)
 H23(1.1257) H25(1.1208) H26(1.257) H27(1.2864) H28(1.1882) H29(1.0569)
 H31(0.9945) H32(0.989) H33(0.9708) H34(0.9492) H35(0.957) H37(0.7813)
 H38(0.665) H39(0.6983) H40(0.8486) H41(0.9635) H1SA(0.5475) H1SB(0.4737)
 H2SA(0.4139) H2SB(0.4858) H2SC(0.4124) H3SA(0.5998) H3SB(0.6751) H4SA(0.7187)
 H4SB(0.6315) H4SC(0.7071) H5SA(0.8005) H5SB(0.8576) H6SA(0.784) H6SB(0.8341)
 H6SC(0.8913) H7SA(0.9714) H7SB(0.9304) H8SA(1.0919) H8SB(1.102) H8SC(1.0614)
;
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_submission_special_instructions 'No special instructions were received'