Molybdenum and tungsten complexes with carbon dioxide and ethylene ligands
Álvarez, María; Galindo, Agustín; Pérez, Pedro J.; Carmona, Ernesto; Chemical Science 10 (2019) 8541–; doi:10.1039/C9SC03225H

data_1555287
_publ_section_title
;
 Molybdenum and tungsten complexes with carbon dioxide and ethylene
 ligands
;
_journal_issue                   37
_journal_name_full               'Chemical Science'
_journal_page_first              8541
_journal_paper_doi               10.1039/C9SC03225H
_journal_volume                  10
_journal_year                    2019
_chemical_formula_moiety         'C35 H31 Mo N O2 P2, 2(C4 H8 O)'
_chemical_formula_sum            'C43 H47 Mo N O4 P2'
_chemical_formula_weight         799.69
_chemical_properties_physical
'air-sensitive, moisture-sensitive,Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-12-08
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_audit_update_record
;
2019-04-23 deposited with the CCDC.	2019-08-13 downloaded from the CCDC.
;
_cell_angle_alpha                100.120(4)
_cell_angle_beta                 101.056(4)
_cell_angle_gamma                90.987(4)
_cell_formula_units_Z            2
_cell_length_a                   11.1529(10)
_cell_length_b                   12.0142(12)
_cell_length_c                   14.6450(15)
_cell_measurement_reflns_used    9717
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.44
_cell_volume                     1893.3(3)
_computing_cell_refinement       'Bruker Apex3, 2016'
_computing_data_collection       'Bruker Apex3, 2016'
_computing_data_reduction        'SAINT v8.35A (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Fixed Chi'
_diffrn_measurement_device_type  'Bruker D8 Quest CCD Apex3'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0885
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            133684
_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         26.021
_diffrn_reflns_theta_min         2.118
_diffrn_source                   'microfocus sealed x-ray tube'
_diffrn_source_type              'Incoatec I/mS high brilliance'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.475
_exptl_absorpt_correction_T_max  0.3334
_exptl_absorpt_correction_T_min  0.2814
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1191 before and 0.0809 after correction.
The Ratio of minimum to maximum transmission is 0.8440.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_description       Block
_exptl_crystal_F_000             832
_exptl_crystal_recrystallization_method
'Recrystallised from a mixture of THF and petroleum ether by slow cooling'
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.579
_refine_diff_density_min         -1.325
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         7458
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0399
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0706P)^2^+1.8863P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1047
_refine_ls_wR_factor_ref         0.1098
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6552
_reflns_number_total             7458
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc03225h2.cif
_cod_data_source_block           compound_2a
_cod_database_code               1555287
_shelx_estimated_absorpt_t_max   0.959
_shelx_estimated_absorpt_t_min   0.915
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C51-C50 \\sim C50-C49 \\sim C49-C48
 with sigma of 0.02
 O47-C51 \\sim O47-C48
 with sigma of 0.02
 O47-C50 \\sim O47-C49
 with sigma of 0.04
 C50-C48 \\sim C51-C49
 with sigma of 0.04
 C51B-C50B \\sim C50B-C49B \\sim C49B-C48B
 with sigma of 0.02
 O47B-C51B \\sim O47B-C48B
 with sigma of 0.02
 O47B-C50B \\sim O47B-C49B
 with sigma of 0.04
 C50B-C48B \\sim C51B-C49B
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O47 \\sim C48 \\sim C49 \\sim C50 \\sim C51: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
O47B \\sim C48B \\sim C49B \\sim C50B \\sim C51B: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 O47, C48, C49, C50, C51
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O47B, C48B, C49B, C50B, C51B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O47B)=Sof(C48B)=Sof(H48C)=Sof(H48D)=Sof(C49B)=Sof(H49C)=Sof(H49D)=
 Sof(C50B)=Sof(H50C)=Sof(H50D)=Sof(C51B)=Sof(H51C)=Sof(H51D)=1-FVAR(1)
 Sof(O47)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(C50)=
 Sof(H50A)=Sof(H50B)=Sof(C51)=Sof(H51A)=Sof(H51B)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C48(H48A,
 H48B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B), C43(H43A,H43B),
 C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C48B(H48C,H48D), C49B(H49C,
 H49D), C50B(H50C,H50D), C51B(H51C,H51D)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C16(H16), C17(H17), C18(H18), C31(H31), C32(H32), C33(H33), C34(H34),
  C35(H35), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41)
;
_shelx_shelxl_version_number     2014/7
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a 100 micro/m MITIGEN holder oil'
_olex2_submission_special_instructions 'No special instructions were received'