Utilising an anilido-imino ligand to stabilise zinc-phosphanide complexes: reactivity and fluorescent properties.
Webb, Dylan; Fulton, J. Robin; Dalton transactions (Cambridge, England : 2003) 48 (2019) 8094–8105; doi:10.1039/c9dt00681h

data_7049727
_publ_section_title
;
 Utilising an anilido-imino ligand to stabilise zinc-phosphanide
 complexes: reactivity and fluorescent properties.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8094
_journal_page_last               8105
_journal_paper_doi               10.1039/c9dt00681h
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         '2(C38 H59 N3 Si2 Zn)'
_chemical_formula_sum            'C76 H118 N6 Si4 Zn2'
_chemical_formula_weight         1358.86
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-27
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-14 deposited with the CCDC.    2019-04-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.1072(2)
_cell_length_b                   19.7437(3)
_cell_length_c                   21.5080(3)
_cell_measurement_reflns_used    20840
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      71.6950
_cell_measurement_theta_min      3.9080
_cell_volume                     7689.18(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0856
_diffrn_detector_type            EosS2
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_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   41.00   66.00   1.0000    2.7100
omega____ theta____ kappa____ phi______ frames
    -       36.0104   77.0000 -120.0000 25

  2 omega   73.00   99.00   1.0000    2.7100
omega____ theta____ kappa____ phi______ frames
    -       36.0104   77.0000 -120.0000 26

  3 omega  101.00  126.00   1.0000   10.8400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000 -180.0000 25

  4 omega  139.00  177.00   1.0000   10.8400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000 -180.0000 38

  5 omega  118.00  175.00   1.0000   10.8400
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  -90.0000 57

  6 omega  136.00  161.00   1.0000   10.8400
omega____ theta____ kappa____ phi______ frames
    -      108.0000   12.0000    0.0000 25

  7 omega  137.00  163.00   1.0000   10.8400
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000   60.0000 26

  8 omega  144.00  173.00   1.0000   10.8400
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000   30.0000 29

  9 omega  119.00  170.00   1.0000   10.8400
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 51

 10 omega   90.00  116.00   1.0000   10.8400
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000   30.0000 26

 11 omega   57.00   92.00   1.0000   10.8400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000    0.0000 35

 12 omega   80.00  130.00   1.0000   10.8400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000    0.0000 50

 13 omega  117.00  142.00   1.0000   10.8400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -91.0000  120.0000 25

 14 omega   47.00   93.00   1.0000   10.8400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000   90.0000 46

 15 omega   49.00   76.00   1.0000   10.8400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  150.0000 27

 16 omega   40.00   79.00   1.0000   10.8400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000   60.0000 39

 17 omega   41.00   76.00   1.0000   10.8400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000  -30.0000 35

 18 omega   39.00   89.00   1.0000   10.8400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000  -90.0000 50

 19 omega   39.00   64.00   1.0000   10.8400
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  -30.0000 25

 20 omega   26.00   53.00   1.0000    2.7100
omega____ theta____ kappa____ phi______ frames
    -       36.0104  -99.0000 -150.0000 27

 21 omega  -34.00   62.00   1.0000    2.7100
omega____ theta____ kappa____ phi______ frames
    -       36.0104  -19.0000  -90.0000 96

 22 omega   92.00  140.00   1.0000   10.8400
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000 -180.0000 48

 23 omega  120.00  145.00   1.0000   10.8400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000 -120.0000 25

 24 omega   20.00   67.00   1.0000    2.7100
omega____ theta____ kappa____ phi______ frames
    -       36.0104   57.0000  150.0000 47

 25 omega   12.00   70.00   1.0000    2.7100
omega____ theta____ kappa____ phi______ frames
    -       36.0104   77.0000   60.0000 58

 26 omega  -34.00   -5.00   1.0000    2.7100
omega____ theta____ kappa____ phi______ frames
    -       36.0104  -19.0000    0.0000 29
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0214778000
_diffrn_orient_matrix_UB_12      0.0073829000
_diffrn_orient_matrix_UB_13      -0.0690129000
_diffrn_orient_matrix_UB_21      0.0660204000
_diffrn_orient_matrix_UB_22      -0.0448120000
_diffrn_orient_matrix_UB_23      -0.0186465000
_diffrn_orient_matrix_UB_31      -0.0491706000
_diffrn_orient_matrix_UB_32      -0.0633995000
_diffrn_orient_matrix_UB_33      0.0050984000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0205
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            34922
_diffrn_reflns_point_group_measured_fraction_full 0.922
_diffrn_reflns_point_group_measured_fraction_max 0.909
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.770
_diffrn_reflns_theta_min         4.682
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.686
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.973
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_description       prism
_exptl_crystal_F_000             2928
_exptl_crystal_size_max          0.1931
_exptl_crystal_size_mid          0.1713
_exptl_crystal_size_min          0.0946
_refine_diff_density_max         0.349
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details
;
 Flack x determined using 5493 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.009(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     823
_refine_ls_number_reflns         13699
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0248
_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^)+(0.0376P)^2^+1.2065P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0650
_refine_ls_wR_factor_ref         0.0660
_reflns_Friedel_coverage         0.770
_reflns_Friedel_fraction_full    0.840
_reflns_Friedel_fraction_max     0.815
_reflns_number_gt                13180
_reflns_number_total             13699
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00681h2.cif
_cod_data_source_block           Compound-2
_cod_depositor_comments
'Adding full bibliography for 7049727--7049732.cif.'
_cod_database_code               7049727
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C38 H59 N3 Si2 Zn'
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
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 Ternary CH refined with riding coordinates:
 C68(H68), C30(H30), C65(H65), C18(H18), C56(H56), C15(H15), C53(H53), C27(H27)
2.b Aromatic/amide H refined with riding coordinates:
 C51(H51), C25(H25), C12(H12), C24(H24), C43(H43), C7(H7), C46(H46), C61(H61),
 C8(H8), C11(H11), C44(H44), C6(H6), C63(H63), C45(H45), C49(H49), C5(H5),
 C13(H13), C23(H23), C62(H62), C50(H50)
2.c Idealised Me refined as rotating group:
 C76(H76A,H76B,H76C), C36(H36A,H36B,H36C), C66(H66A,H66B,H66C), C55(H55A,H55B,
 H55C), C42(H42A,H42B,H42C), C4(H4A,H4B,H4C), C35(H35A,H35B,H35C), C38(H38A,
 H38B,H38C), C71(H71A,H71B,H71C), C37(H37A,H37B,H37C), C75(H75A,H75B,H75C),
 C54(H54A,H54B,H54C), C74(H74A,H74B,H74C), C28(H28A,H28B,H28C), C32(H32A,H32B,
 H32C), C31(H31A,H31B,H31C), C57(H57A,H57B,H57C), C16(H16A,H16B,H16C), C69(H69A,
 H69B,H69C), C33(H33A,H33B,H33C), C20(H20A,H20B,H20C), C17(H17A,H17B,H17C),
 C19(H19A,H19B,H19C), C72(H72A,H72B,H72C), C67(H67A,H67B,H67C), C73(H73A,H73B,
 H73C), C70(H70A,H70B,H70C), C34(H34A,H34B,H34C), C58(H58A,H58B,H58C), C29(H29A,
 H29B,H29C)
;
_shelx_res_checksum              51003
_olex2_submission_special_instructions 'No special instructions were received'