Crystal structure of hexacarbonyl-(μ2-methanoato-k2 O:O′)-(μ2–bis(di-p-tolylphosphino)cyclohexylamine-κ2 P:P′)dirhenium(I), C42H45NO8P2Re2
Kama, Dumisani V.; Brink, Alice; Alberto, Roger; Roodt, Andreas; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 303–305; doi:10.1515/ncrs-2019-0632

data_8105090
_publ_section_title
;
 Crystal structure of hexacarbonyl-(\m2-methanoato-k2
 O:O&#x2032;)-(\m2--bis(di-p-tolylphosphino)cyclohexylamine-\k2
 P:P&#x2032;)dirhenium(I), C42H45NO8P2Re2
;
_journal_issue                   2
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              303
_journal_page_last               305
_journal_paper_doi               10.1515/ncrs-2019-0632
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C42 H45 N O8 P2 Re2'
_chemical_formula_sum            'C42 H45 N O8 P2 Re2'
_chemical_formula_weight         1126.13
_chemical_name_systematic
;
<i>fac</i>-bis(hexacarbonyl-<i>\m</i>~2~-methoxy)(<i>\m</i>~2~-
bis(di-<i>p</i>-tolylphosphino) cyclohexylamine)dirhenium(I)
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 121.383(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.1612(7)
_cell_length_b                   13.0229(3)
_cell_length_c                   14.9180(4)
_cell_measurement_reflns_used    4842
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      32.631
_cell_measurement_theta_min      2.791
_cell_volume                     4007.2(2)
_computing_cell_refinement       'CrysAlis^Pro^, Ver. 1.171.37.31 [1]'
_computing_data_collection       'CrysAlis^Pro^, Ver. 1.171.37.31 [1]'
_computing_data_reduction        'CrysAlis^Pro^, Ver. 1.171.37.31 [1]'
_computing_molecular_graphics    'Diamond 3.2 [4]'
_computing_publication_material  'Olex2-2009 [5]'
_computing_structure_refinement  'SHELXL-2018/3 [3]'
_computing_structure_solution    'SHELXT-2018/2 [2]'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4498
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20362
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         2.748
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.170
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,

Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)

(compiled Jan 14 2014,18:38:05)

Empirical absorption correction using spherical harmonics,

 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.867
_exptl_crystal_description       cube
_exptl_crystal_F_000             2192
_exptl_crystal_size_max          0.301
_exptl_crystal_size_mid          0.219
_exptl_crystal_size_min          0.101
_refine_diff_density_max         0.877
_refine_diff_density_min         -1.005
_refine_diff_density_rms         0.129
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         4842
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0235
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0258P)^2^+3.2472P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0553
_refine_ls_wR_factor_ref         0.0596
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4325
_reflns_number_total             4842
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2019-0632_suppl.cif
_cod_data_source_block           exp_1115
_cod_database_code               8105090
_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
 Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C3)=Sof(H3A)=Sof(H3B)=1-FVAR(1)
 Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C6)=Sof(H6A)=Sof(H6B)=FVAR(1)
 Fixed Sof: C1(0.5) H1(0.5) C4(0.5) H4A(0.5) H4B(0.5)
3.a Ternary CH refined with riding coordinates:
 C1(H1)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B)
3.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C15(H15), C16(H16), C22(H22), C23(H23), C25(H25), C26(H26)
3.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C17(H17A,H17B,H17C), C27(H27A,H27B,H27C)
;