Accessing Multimetallic Complexes with a Phosphorus(I) Zwitterion
Kosnik, Stephanie C.; Nascimento, Maxemilian C.; Binder, Justin Frank; Macdonald, Charles L. B.; Dalton Transactions  (2017) –; doi:10.1039/C7DT03844E

data_7044842
_publ_section_title
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 Accessing Multimetallic Complexes with a Phosphorus(I) Zwitterion
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C7DT03844E
_journal_year                    2017
_chemical_formula_moiety         'C38 H31 O5 P3 W'
_chemical_formula_sum            'C38 H31 O5 P3 W'
_chemical_formula_weight         844.39
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-07-28
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
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_audit_update_record
;
2017-10-06 deposited with the CCDC.
2017-11-22 downloaded from the CCDC.
;
_cell_angle_alpha                91.631(3)
_cell_angle_beta                 100.807(3)
_cell_angle_gamma                114.414(3)
_cell_formula_units_Z            2
_cell_length_a                   11.3304(11)
_cell_length_b                   11.7799(11)
_cell_length_c                   15.1089(14)
_cell_measurement_reflns_used    9352
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      29.00
_cell_measurement_theta_min      3.05
_cell_volume                     1791.0(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XH (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      170.19
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0605
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            89946
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.224
_diffrn_reflns_theta_min         3.048
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.400
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5269
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1178 before and 0.0655 after correction.
The Ratio of minimum to maximum transmission is 0.7065.
The \l/2 correction factor is Not present.
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_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_description       Plate
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.351
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.034
_refine_diff_density_max         4.111
_refine_diff_density_min         -1.374
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         9717
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0397P)^2^+4.4580P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0898
_refine_ls_wR_factor_ref         0.0938
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8444
_reflns_number_total             9717
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03844e2.cif
_cod_data_source_block           shelx_CCDC6
_cod_database_code               7044842
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.893
_shelx_estimated_absorpt_t_min   0.382
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C22(H22),
 C23(H23), C24(H24), C25(H25), C26(H26), C32(H32), C33(H33), C34(H34), C35(H35),
  C36(H36), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46)
2.b Idealised Me refined as rotating group:
 C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C)
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_olex2_submission_special_instructions 'No special instructions were received'