An isolable magnesium diphosphaethynolate complex.
Gilliard, Robert J.; Heift, Dominikus; Benkő, Zoltán; Keiser, Jerod M.; Rheingold, Arnold L.; Grützmacher, Hansjörg; Protasiewicz, John D.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 666–669; doi:10.1039/c7dt04539e

data_7044980
_publ_section_title
;
 An isolable magnesium diphosphaethynolate complex.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              666
_journal_page_last               669
_journal_paper_doi               10.1039/c7dt04539e
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C18 H32 Mg O6 P2'
_chemical_formula_sum            'C18 H32 Mg O6 P2'
_chemical_formula_weight         430.68
_chemical_name_systematic        '[(THF)4Mg(OCP)2]'
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2016-02-17
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.02.16 svn.r3264 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-04-19 deposited with the CCDC.
2017-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.837(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.5504(9)
_cell_length_b                   14.2261(19)
_cell_length_c                   11.0598(10)
_cell_measurement_reflns_used    1751
_cell_measurement_temperature    225
_cell_measurement_theta_max      23.748
_cell_measurement_theta_min      2.722
_cell_volume                     1176.9(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2013.6-2 (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, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2008)'
_diffrn_ambient_temperature      225
_diffrn_detector                 'Bruker APEX CCD'
_diffrn_detector_area_resol_mean 8.0
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_Laue_measured_fraction_full 0.932
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6606
_diffrn_reflns_point_group_measured_fraction_full 0.932
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.440
_diffrn_reflns_theta_min         2.723
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.239
_exptl_absorpt_correction_T_max  0.6462
_exptl_absorpt_correction_T_min  0.5525
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0481 before and 0.0405 after correction.
The Ratio of minimum to maximum transmission is 0.8550.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_description       block
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.206
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         2166
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0452
_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^)+(0.0570P)^2^+0.2570P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1085
_refine_ls_wR_factor_ref         0.1261
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1425
_reflns_number_total             2166
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04539e2.cif
_cod_data_source_block           pro61_a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7044980--7044981.cif.
;
_cod_database_code               7044980
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.938
_shelx_estimated_absorpt_t_min   0.932
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Rigid body (RIGU) restrains
 C007, C008, C009, C00A, C2, C0AA, C1AA, C1, C2A, C1AB, C0AB, C1A, C0, C00B,
 C3, C4, O004, O003
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(C1AB)=Sof(H1AC)=Sof(H1AD)=Sof(C0AB)=
 Sof(H0AC)=Sof(H0AD)=Sof(C1A)=Sof(H1AE)=Sof(H1AF)=1-FVAR(1)
 Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C0AA)=Sof(H0AA)=Sof(H0AB)=Sof(C1AA)=Sof(H1AA)=
 Sof(H1AB)=Sof(C1)=Sof(H1A)=Sof(H1B)=FVAR(1)
 Sof(C0)=Sof(H0A)=Sof(H0B)=Sof(C00B)=Sof(H00I)=Sof(H00J)=Sof(C3)=Sof(H3A)=
 Sof(H3B)=Sof(C4)=Sof(H4A)=Sof(H4B)=1-FVAR(2)
 Sof(C007)=Sof(H00A)=Sof(H00B)=Sof(C008)=Sof(H00C)=Sof(H00D)=Sof(C009)=
 Sof(H00E)=Sof(H00F)=Sof(C00A)=Sof(H00G)=Sof(H00H)=FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
 C007(H00A,H00B), C008(H00C,H00D), C009(H00E,H00F), C00A(H00G,H00H), C2(H2A,
 H2B), C0AA(H0AA,H0AB), C1AA(H1AA,H1AB), C1(H1A,H1B), C2A(H2AA,H2AB), C1AB(H1AC,
 H1AD), C0AB(H0AC,H0AD), C1A(H1AE,H1AF), C0(H0A,H0B), C00B(H00I,H00J), C3(H3A,
 H3B), C4(H4A,H4B)
;
_shelx_res_checksum              15223
_olex2_submission_special_instructions 'No special instructions were received'