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_1555288
_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         'C36 H35 N O2 P2 W, 2(C H2 Cl2)'
_chemical_formula_sum            'C38 H39 Cl4 N O2 P2 W'
_chemical_formula_weight         929.29
_chemical_properties_physical
'air-sensitive, moisture-sensitive,Air-sensitive,Moisture-sensitive'
_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
_audit_update_record
;
2019-04-23 deposited with the CCDC.	2019-08-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.571(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   35.714(3)
_cell_length_b                   16.0980(13)
_cell_length_c                   15.0574(12)
_cell_measurement_reflns_used    9869
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      25.14
_cell_measurement_theta_min      2.23
_cell_volume                     8050.6(11)
_computing_cell_refinement       'Bruker Apex3, 2017'
_computing_data_collection       'Bruker Apex3, 2017'
_computing_data_reduction        'SAINT v8.38A (Bruker, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2014)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'Bruker D8 Quest'
_diffrn_measurement_device_type  'Bruker D8 Quest'
_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  0.0642
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            127331
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.178
_diffrn_reflns_theta_max         25.178
_diffrn_reflns_theta_min         2.179
_diffrn_source                   'microfocus sealed x-ray tube'
_diffrn_source_type              'Incoatec I/mS high brilliance'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.247
_exptl_absorpt_correction_T_max  0.0183
_exptl_absorpt_correction_T_min  0.0046
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1099 before and 0.0732 after correction. 
The Ratio of minimum to maximum transmission is 0.2514. 
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_description       prism
_exptl_crystal_F_000             3696
_exptl_crystal_recrystallization_method 'Crystallised from dichloromethane'
_exptl_crystal_size_max          0.315
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.909
_refine_diff_density_min         -1.871
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.192
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         7184
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.194
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0677
_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^)+(0.0134P)^2^+268.4964P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1481
_refine_ls_wR_factor_ref         0.1560
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6058
_reflns_number_total             7184
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc03225h2.cif
_cod_data_source_block           compound_3b
_cod_original_cell_volume        8050.5(11)
_cod_original_sg_symbol_Hall     '-C 2yn'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1555288
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl4-C37 = Cl3-C37
 1.771 with sigma of 0.01
 Cl4-Cl3
 2.916 with sigma of 0.03
3. Uiso/Uaniso restraints and constraints
Cl3 \\sim Cl4 \\sim C37: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
4. Rigid body (RIGU) restrains
 Cl3, Cl4, C37
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C12(H12A,
 H12B), C38(H38A,H38B), C37(H37A,H37B)
5.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18),
 C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28),
  C29(H29), C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36)
;
_smtbx_masks_special_details
;
During the structure refinement, regions of electron density 
were identified as a highly disordered dichloromethane solvent molecules. 
Attempts to model these electron densities as dichloromethane 
were not successful due to the extent of the disorder. 
In the final structure model, this electron density contribution
has been removed from the intensity data
using the solvent mask tool in Olex2 (Dolomanov, O.V., Bourhis, 
L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.(2009), J. Appl.
Cryst. 42, 339-341.)
;
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a 200 micro/m MITEGEN holder in perfluoroether oil'