Diolefins with an ether/thioether functionality as ligands in the coordination sphere of Ni and Rh.
Lichtenberg, Crispin; Bloch, Jan; Gianetti, Thomas L.; Büttner, Torsten; Geier, Jens; Grützmacher, Hansjörg; Dalton transactions (Cambridge, England : 2003) 44 (2015) 20056–20066; doi:10.1039/c5dt03279b

data_7037061
_publ_section_title
;
 Diolefins with an ether/thioether functionality as ligands in the
 coordination sphere of Ni and Rh.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              20056
_journal_page_last               20066
_journal_paper_doi               10.1039/c5dt03279b
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C48 H37 Ni O P, 2(C4 H8 O)'
_chemical_formula_sum            'C56 H53 Ni O3 P'
_chemical_formula_weight         863.66
_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     iterative
_audit_creation_date             2015-05-12
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-08-24 deposited with the CCDC.
2015-10-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.427(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6848(11)
_cell_length_b                   13.0667(15)
_cell_length_c                   34.253(4)
_cell_measurement_reflns_used    6985
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.80
_cell_measurement_theta_min      2.25
_cell_volume                     4315.2(9)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_av_unetI/netI     0.0522
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            40104
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.972
_diffrn_reflns_theta_min         1.194
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.533
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6561
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0883 before and 0.0542 after correction.
The Ratio of minimum to maximum transmission is 0.8801.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_description       needle
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.946
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     546
_refine_ls_number_reflns         9390
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.946
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0820P)^2^+4.5600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1234
_refine_ls_wR_factor_ref         0.1393
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7201
_reflns_number_total             9390
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03279b2.cif
_cod_data_source_block           Compound5
_cod_depositor_comments
'Adding full bibliography for 7037058--7037062.cif.'
_cod_database_code               7037061
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Sof(C55)=Sof(H55C)=Sof(H55D)=Sof(C56)=Sof(H56C)=Sof(H56D)=Sof(O3)=Sof(C54)=
 Sof(H54C)=Sof(H54D)=Sof(C53)=Sof(H53C)=Sof(H53D)=1-FVAR(1)
 Sof(C53A)=Sof(H53A)=Sof(H53B)=Sof(O3A)=Sof(C56A)=Sof(H56A)=Sof(H56B)=
 Sof(C55A)=Sof(H55A)=Sof(H55B)=Sof(C54A)=Sof(H54A)=Sof(H54B)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C1(H1), C5(H5), C20(H20), C4(H4), C16(H16), C19(H19)
3.b Secondary CH2 refined with riding coordinates:
 C50(H50A,H50B), C49(H49A,H49B), C52(H52A,H52B), C51(H51A,H51B), C53A(H53A,
 H53B), C56A(H56A,H56B), C55A(H55A,H55B), C55(H55C,H55D), C56(H56C,H56D),
 C54(H54C,H54D), C53(H53C,H53D), C54A(H54A,H54B)
3.c Aromatic/amide H refined with riding coordinates:
 C23(H23), C11(H11), C29(H29), C15(H15), C48(H48), C25(H25), C44(H44),
 C47(H47), C41(H41), C26(H26), C24(H24), C45(H45), C46(H46), C13(H13), C14(H14),
  C33(H33), C28(H28), C34(H34), C27(H27), C9(H9), C12(H12), C40(H40), C38(H38),
 C30(H30), C42(H42), C39(H39), C8(H8), C35(H35), C36(H36), C10(H10), C32(H32)
;
_shelx_res_checksum              9482
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'